CN111875977B - Permanent violet refining system and refining method - Google Patents
Permanent violet refining system and refining method Download PDFInfo
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- CN111875977B CN111875977B CN202010879158.6A CN202010879158A CN111875977B CN 111875977 B CN111875977 B CN 111875977B CN 202010879158 A CN202010879158 A CN 202010879158A CN 111875977 B CN111875977 B CN 111875977B
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- dichlorobenzene
- washing
- permanent violet
- steam
- distillation
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- CGLVZFOCZLHKOH-UHFFFAOYSA-N 8,18-dichloro-5,15-diethyl-5,15-dihydrodiindolo(3,2-b:3',2'-m)triphenodioxazine Chemical compound CCN1C2=CC=CC=C2C2=C1C=C1OC3=C(Cl)C4=NC(C=C5C6=CC=CC=C6N(C5=C5)CC)=C5OC4=C(Cl)C3=NC1=C2 CGLVZFOCZLHKOH-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000007670 refining Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims abstract description 271
- 238000005406 washing Methods 0.000 claims abstract description 103
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 101
- 238000004821 distillation Methods 0.000 claims abstract description 59
- 239000000047 product Substances 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 14
- 238000004537 pulping Methods 0.000 claims abstract description 10
- 238000011085 pressure filtration Methods 0.000 claims abstract description 5
- 238000001256 steam distillation Methods 0.000 claims description 38
- 238000007599 discharging Methods 0.000 claims description 34
- 239000012452 mother liquor Substances 0.000 claims description 34
- 238000003825 pressing Methods 0.000 claims description 20
- 239000012065 filter cake Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 12
- 238000011084 recovery Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 11
- 239000002002 slurry Substances 0.000 abstract description 8
- LWEAHXKXKDCSIE-UHFFFAOYSA-M 2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 LWEAHXKXKDCSIE-UHFFFAOYSA-M 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 abstract description 5
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000008236 heating water Substances 0.000 abstract description 3
- 238000010533 azeotropic distillation Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- UGNWTBMOAKPKBL-UHFFFAOYSA-N tetrachloro-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(Cl)=C(Cl)C1=O UGNWTBMOAKPKBL-UHFFFAOYSA-N 0.000 description 6
- 238000010009 beating Methods 0.000 description 5
- 238000004065 wastewater treatment Methods 0.000 description 5
- CSKNSYBAZOQPLR-UHFFFAOYSA-N benzenesulfonyl chloride Chemical compound ClS(=O)(=O)C1=CC=CC=C1 CSKNSYBAZOQPLR-UHFFFAOYSA-N 0.000 description 4
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 4
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 description 3
- OPJDPIWCAQORQI-UHFFFAOYSA-N benzenesulfonic acid;n,n-diethylethanamine Chemical compound CC[NH+](CC)CC.[O-]S(=O)(=O)C1=CC=CC=C1 OPJDPIWCAQORQI-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- PLAZXGNBGZYJSA-UHFFFAOYSA-N 9-ethylcarbazole Chemical compound C1=CC=C2N(CC)C3=CC=CC=C3C2=C1 PLAZXGNBGZYJSA-UHFFFAOYSA-N 0.000 description 2
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- DWDURZSYQTXVIN-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-methyliminocyclohexa-2,5-dien-1-ylidene)methyl]aniline Chemical compound C1=CC(=NC)C=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 DWDURZSYQTXVIN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PPSZHCXTGRHULJ-UHFFFAOYSA-N dioxazine Chemical compound O1ON=CC=C1 PPSZHCXTGRHULJ-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B19/00—Oxazine dyes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D498/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms
- C07D498/22—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms in which the condensed system contains four or more hetero rings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a permanent violet refining system and a refining method, and belongs to the technical field of permanent violet production. The system comprises an o-dichlorobenzene washing centrifuge, a water vapor distillation device, a water washing and pressure filtration device and a post-treatment device, wherein the permanent violet crude product is firstly washed by o-dichlorobenzene in the o-dichlorobenzene washing centrifuge, and substances dissolved in the o-dichlorobenzene in the permanent violet crude product are removed. And (3) delivering the centrifugal filter residues to a water vapor distillation device, pulping by heating water, and then introducing steam, wherein on one hand, high temperature is provided to enable o-dichlorobenzene in the centrifugal filter residues to be subjected to azeotropic distillation with water, and on the other hand, the steam provides a certain stripping effect to enable the o-dichlorobenzene to be fully separated out of the centrifugal filter residues, so that the residual of the o-dichlorobenzene in the permanent violet is reduced. The permanent violet slurry is fed into a water washing filter press device for filter press dehydration, and hot water is heated for hot water washing to remove triethylamine hydrochloride. After detection and three times of washing, the residual quantity of the o-dichlorobenzene in the permanent violet finished product is obviously smaller than that of the traditional nekal washing.
Description
Technical Field
The invention belongs to the technical field of permanent violet production, and particularly relates to a permanent violet refining system and a refining method.
Background
The permanent violet RL is a high-grade organic pigment of dioxazine, has outstanding coloring strength and brightness, excellent heat resistance, permeation resistance and good light fastness, has wide application range, and is popular in the fields of paint, plastics, organic glass, rubber, textile printing, solvent ink, water-based ink, package printing and the like.
The main production process of the permanent violet RL comprises the following steps: dissolving carbazole in alkali liquor for alkylation to obtain N-ethylcarbazole, nitrifying N-ethylcarbazole in nitric acid, reducing with H2, condensing in tetrachlorobenzoquinone, finally closing ring in benzenesulfonyl chloride, oxidizing to obtain permanent violet crude liquid, and filtering, drying, pulverizing and other treatment procedures to obtain the product. In actual production, the permanent violet crude liquid is discharged at 120 ℃, the solvent is removed by filtering, the filter cake is washed by o-dichlorobenzene, nekal water and hot water, and finally the filter cake is subjected to filter pressing and drying to obtain a finished product.
The washing process of the permanent violet crude product has the following problems:
firstly, the residual quantity of o-dichlorobenzene is large, and when the plate frame filter pressing and the product are dried, a large amount of waste gas is generated, the environment is polluted, the safety risk exists, and meanwhile, the chemical substances in the product, which affect the final product due to the high residual quantity of o-dichlorobenzene, are safely used and remain, so that the quality of the product is reduced.
Secondly, the use of the nekal as a detergent leads to large discharge capacity of washing wastewater, increased salt content and COD value, and further leads to increased difficulty in wastewater treatment.
Disclosure of Invention
In view of the above, the invention provides a permanent violet refining system to solve the technical problems of large o-dichlorobenzene residue, large wastewater discharge and difficult treatment in the crude permanent violet refining process in the prior art.
The invention also provides a permanent violet refining method.
The technical scheme adopted for solving the technical problems is as follows:
a permanent violet refining system comprising:
an ortho-dichlorobenzene washing centrifuge is provided with an ortho-dichlorobenzene feeding distribution disc;
the steam distillation device comprises a steam distillation kettle and an orthodichlorobenzene recycling component arranged at the top of the steam distillation kettle, wherein the feeding end of the steam distillation kettle is connected with the solid-phase discharging end of the orthodichlorobenzene washing centrifuge, and a hot water feeding pipe and a pulping stirrer are arranged on the steam distillation kettle; the kettle bottom of the water vapor distillation kettle is connected with a water vapor feeding pipe;
the feeding end of the water washing and pressure filtration device is connected with the discharging end of the tower kettle of the water vapor distillation kettle, and the water washing and pressure filtration device is provided with a hot water feeding distribution disc; and
the post-treatment device comprises a filter cake dryer for drying the permanent violet filter cake from the washing filter pressing device and a filter cake pulverizer for pulverizing the permanent violet filter cake.
Preferably, the orthodichlorobenzene recovery assembly comprises a condenser, an orthodichlorobenzene separating tank and a vacuum pump, wherein a hot material inlet section of the condenser is connected with a top gas phase discharge end of the water vapor distillation kettle, the orthodichlorobenzene separating tank is connected with a condensate discharge end of the condenser, and an inlet of the vacuum pump is connected with the orthodichlorobenzene separating tank.
Preferably, a centrifugal mother liquor discharging pipe is arranged on the o-dichlorobenzene washing centrifugal machine, and a centrifugal mother liquor pool is connected to the centrifugal mother liquor discharging pipe.
Preferably, a heating jacket is arranged on the outer side of the steam distillation kettle, and the heating jacket is connected with a heat conduction oil feeding pipe and a heat conduction oil discharging pipe.
Preferably, the water washing filter pressing device is provided with a filtrate discharging pipe, and the filtrate discharging pipe is connected with a filtrate buffer pool.
A permanent violet refining method comprises the following steps:
washing o-dichlorobenzene: washing the crude product of the permanent violet subjected to removal of the o-dichlorobenzene by using the o-dichlorobenzene, and after the o-dichlorobenzene is washed, centrifugally drying to obtain the permanent violet subjected to primary washing;
steam distillation: pulping the primary washing permanent violet, introducing steam into a distillation kettle, and performing steam distillation to remove o-dichlorobenzene to obtain secondary washing permanent violet;
washing with hot water: filtering the secondary washing permanent violet by a filter press, washing a filter cake on the filter press by hot water, and filtering to obtain wet permanent violet;
drying and crushing: drying and crushing wet permanent violet to obtain refined permanent violet.
Preferably, in the step of steam distillation, steam with the temperature of 120-150 ℃ is introduced into a distillation kettle.
Preferably, in the step of hot water washing, the temperature of the hot water is 42 to 60 ℃.
According to the technical scheme, the invention provides a permanent violet refining system and a refining method, which have the beneficial effects that: the method comprises the steps of sequentially arranging an ortho-dichlorobenzene washing centrifuge, a water vapor distillation device, a water washing filter press device and a post-treatment device, removing a permanent violet crude product of ortho-dichlorobenzene, washing with ortho-dichlorobenzene at a certain temperature in the ortho-dichlorobenzene washing centrifuge, and removing substances dissolved in ortho-dichlorobenzene in the permanent violet crude product, especially substances such as nitro compounds, benzenesulfonyl chloride, tetrachlorobenzoquinone, thiophen and the like. And after the o-dichlorobenzene is washed, spin-drying is carried out by the o-dichlorobenzene washing centrifugal machine, collecting and uniformly treating centrifugal mother liquor, delivering the centrifugal filter residues into the water vapor distillation device, pulping by heating water first, and then introducing steam, so that on one hand, high temperature is provided to enable o-dichlorobenzene contained in the centrifugal filter residues to be subjected to azeotropic distillation with water, and on the other hand, the steam provides a certain stripping effect to enable the o-dichlorobenzene to be fully separated out of the centrifugal filter residues, thereby effectively removing o-dichlorobenzene components in the centrifugal filter residues and reducing the residual of the o-dichlorobenzene in the permanent violet. After the steam distillation is finished, the permanent violet slurry is sent into the water washing filter pressing device for filter pressing dehydration, and meanwhile, hot water is continuously heated for hot water washing to remove triethylamine hydrochloride in the permanent violet, so that a high-quality permanent violet finished product is obtained. After detection and three times of washing, the residual quantity of the o-dichlorobenzene in the permanent violet finished product is less than 500mg/kg and is far less than that of the traditional powder pulling washing (8000-10000 mg/kg of the o-dichlorobenzene in the traditional powder pulling washing), compared with the traditional process, the residual quantity of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanently fixed purple washing wastewater does not contain a powder pulling material, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is conveniently recovered from the wastewater, and the difficulty of wastewater treatment is reduced.
Drawings
FIG. 1 is a schematic flow diagram of a permanent violet refining system.
In the figure: the permanent violet refining system 10, the ortho-dichlorobenzene washing centrifuge 100, the ortho-dichlorobenzene feeding distribution plate 110, the centrifugal mother liquor discharging pipe 120, the centrifugal mother liquor pond 130, the steam distillation kettle 210, the hot water feeding pipe 211, the beating stirrer 212, the steam feeding pipe 213, the heating jacket 214, the heat conducting oil feeding pipe 2141, the heat conducting oil discharging pipe 2142, the condenser 221, the ortho-dichlorobenzene separating tank 222, the vacuum pump 223, the water washing filter press 300, the hot water feeding distribution plate 310, the filtrate discharging pipe 320, the filtrate buffer tank 321, the filter cake dryer 410, the filter cake crusher 420, the decompression distillation kettle 511, the centrifugal mother liquor feeding pipe 5111, the slag water mixture discharging pipe 5112, the steam feeding pipe 5113, the recovery condenser 5121, the first condensate receiving tank 5122, the negative pressure generating member 5123, the slag discharging pond 513, the permanent violet pulping kettle 521, the permanent violet filter 522 and the first ortho-dichlorobenzene feeding pipe 5211.
Detailed Description
The technical scheme and technical effects of the present invention are further elaborated below in conjunction with the drawings of the present invention.
Referring to FIG. 1, in one embodiment, a system 10 for refining crude permanent violet is provided. Comprising the following steps: the device comprises an ortho-dichlorobenzene washing centrifuge 100, a water vapor distillation device, a water washing filter pressing device 300 and a post-treatment device, wherein an ortho-dichlorobenzene feeding distribution disc 110 is arranged on the ortho-dichlorobenzene washing centrifuge 100.
The steam distillation device comprises a steam distillation kettle 210 and an o-dichlorobenzene recycling component arranged at the top of the steam distillation kettle 210, wherein a feeding end of the steam distillation kettle 210 is connected with a solid-phase discharging end of the o-dichlorobenzene washing centrifuge 100, and a hot water feeding pipe 211 and a pulping stirrer 212 are arranged on the steam distillation kettle 210. The kettle bottom of the steam distillation kettle 210 is connected with a steam feeding pipe 213. The feeding end of the water washing and filter pressing device 300 is connected with the discharging end of the water vapor distillation kettle 210, and the water washing and filter pressing device 300 is provided with a hot water feeding distribution disc 310. The post-treatment device includes a cake dryer 410 for drying the permanent violet filter cake from the water washing filter press 300 and a cake crusher 420 for crushing the permanent violet filter cake.
The method comprises the steps of removing the crude permanent violet of the o-dichlorobenzene, firstly, introducing a certain flow of o-dichlorobenzene into an o-dichlorobenzene washing centrifuge 100 at a certain temperature through an o-dichlorobenzene feeding distribution disc 110, washing the crude permanent violet with the o-dichlorobenzene, and removing substances dissolved in the o-dichlorobenzene, in particular substances such as nitro substances, benzenesulfonyl chloride, tetrachlorobenzoquinone, phenylthiol and the like in the crude permanent violet. After the o-dichlorobenzene is washed, the o-dichlorobenzene is dried by the o-dichlorobenzene washing centrifugal machine 100, centrifugal mother liquor is collected and treated uniformly, centrifugal filter residues are sent into the water vapor distillation device, water is firstly heated into the water vapor distillation kettle 210 through the hot water feeding pipe 211, and the beating stirrer 212 is started to perform beating. Steam is introduced into the steam distillation still 210 through the steam feed pipe 213, for example, steam with a temperature of 120-150 ℃ is introduced, on one hand, high temperature is provided to make o-dichlorobenzene contained in the centrifugal filter residue azeotropically distill with water, and on the other hand, due to the stripping action provided by the steam, o-dichlorobenzene is fully separated out of the centrifugal filter residue, so that the o-dichlorobenzene component in the centrifugal filter residue is effectively removed, and the residual of o-dichlorobenzene in the permanent violet is reduced. After the steam distillation is finished, the permanent violet slurry is sent into the water washing filter pressing device 300 for filter pressing dehydration, and meanwhile, hot water is continuously heated into the water washing filter pressing device 300 through the hot water feeding distribution plate 310 for hot water washing, so that impurity components, such as triethylamine hydrochloride, in the permanent violet, which are soluble in hot water are removed, and a high-quality permanent violet finished product is obtained.
After detection and three times of washing, the residual quantity of the o-dichlorobenzene in the permanent violet finished product is less than 500mg/kg and is far less than that of the traditional powder pulling washing (8000-10000 mg/kg of the o-dichlorobenzene in the traditional powder pulling washing), compared with the traditional process, the residual quantity of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanently fixed purple washing wastewater does not contain a powder pulling material, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is conveniently recovered from the wastewater, and the difficulty of wastewater treatment is reduced.
In an embodiment, the orthodichlorobenzene recycling component comprises a condenser 221, an orthodichlorobenzene separating tank 222 and a vacuum pump 223, wherein a hot material inlet section of the condenser 221 is connected with a top gas phase discharge end of the water vapor distillation kettle 210, the orthodichlorobenzene separating tank 222 is connected with a condensate discharge end of the condenser 221, and an inlet of the vacuum pump 223 is connected with the orthodichlorobenzene separating tank 222. Under the action of the vacuum pump 223, the pressure at the top of the water vapor distillation still 210 is maintained to be 40 KPaA-60 KPaA (KPaA represents absolute pressure unit), water and o-dichlorobenzene are azeotroped, gas phase passes through the bottom of the water vapor distillation still 210 and enters the condenser 221 to be condensed, condensate automatically flows into the o-dichlorobenzene separating tank 222, water and o-dichlorobenzene are layered, and o-dichlorobenzene is recovered.
In yet another embodiment, the ortho-dichlorobenzene washing centrifuge 100 is provided with a centrifugal mother liquor discharging pipe 120, and the centrifugal mother liquor discharging pipe 120 is connected with a centrifugal mother liquor pool 130. And the centrifugal mother liquor which is centrifugally separated by the o-dichlorobenzene washing centrifugal machine 100 and contains a large amount of o-dichlorobenzene enters the centrifugal mother liquor pond 130 through the centrifugal mother liquor discharging pipe 120, and the o-dichlorobenzene components in the centrifugal mother liquor are collected and intensively treated to be recovered.
In one embodiment, the permanent violet refining system 10 further comprises a centrifugal mother liquor treatment unit, wherein the centrifugal mother liquor treatment unit comprises an ortho-dichlorobenzene extraction device and a permanent violet recovery device.
The ortho-dichlorobenzene extraction device comprises a reduced pressure distillation kettle 511, an ortho-dichlorobenzene extraction component and a deslagging water pond 513, wherein a centrifugal mother liquor feeding pipe 5111 is arranged on the reduced pressure distillation kettle 511, and the centrifugal mother liquor feeding pipe 5111 is connected with the outlet end of the centrifugal mother liquor pond 130.
The bottom of the reduced pressure distillation kettle 511 is provided with a slag-water mixture discharge pipe 5112, and the slag-water mixture discharge pipe 5112 is connected with the slag-water discharge pool 513. The ortho-dichlorobenzene extraction component comprises a recovery condenser 5121 and a first condensate receiving groove 5122, wherein a hot side feeding end of the recovery condenser 5121 is connected with the reduced pressure distillation still 511, the first condensate receiving groove 5122 is connected with a condensate discharging end of the recovery condenser 5121, and a negative pressure generating element 5123 is further connected to the first condensate receiving groove 5122. The reduced pressure distillation still 511 is also connected with a vapor feed pipe 5113.
The permanent violet centrifugal mother liquor is conveyed into the reduced pressure distillation kettle 511 through the centrifugal mother liquor feed pipe 5111, and reduced pressure distillation is performed first. The vacuum degree of the distillation still is controlled to be 40 KPaA-60 KPaA (KPaA represents absolute pressure unit), the still temperature is 80-100 ℃, and reduced pressure distillation is carried out. The o-dichlorobenzene component in the permanent violet centrifugal mother liquor is evaporated, and after the evaporated gas phase is condensed by the recovery condenser 5121, the o-dichlorobenzene with the mass concentration of mainly 70% -80% in the condensate is collected in the first condensate receiving tank 5122 and recycled. Other components (mainly comprising about 35% of permanent violet, about 25% of triethylamine benzenesulfonate and about 20% of chloranil) in the permanent violet centrifugal mother liquor are gradually separated out at the bottom of the reduced pressure distillation kettle 511. After most of the o-dichlorobenzene is distilled out of the system, the remaining components are present in the form of distillation residues in the vacuum distillation pot 511.
After the reduced pressure distillation is finished, the distillation residue mainly contains permanent violet, triethylamine benzenesulfonate, chloranil and a small amount of o-dichlorobenzene component, and steam (namely steam with the pressure of 0.2-0.5 MPa) with the temperature of 120-150 ℃ is introduced into the reduced pressure distillation kettle 511 through the steam feed pipe 5113 to carry out steam distillation. In the distillation process, an azeotropic system of vapor and o-dichlorobenzene is formed, the vapor is assisted by vapor stripping, the vapor carries o-dichlorobenzene vapor to be discharged from a gas phase of the reduced pressure distillation kettle 511, and the vapor is condensed by the recovery condenser 5121, the condensate mainly contains water and o-dichlorobenzene, and the condensate is collected in the first condensate receiving tank 5122, and after oil-water separation, the o-dichlorobenzene is recycled. Meanwhile, the steam is condensed, salts (such as triethylamine benzenesulfonate salt) contained in the distillation residues are dissolved in the condensate and form slurry with insoluble components (such as permanent violet) in the distillation residues, so that the distillation residues can be smoothly discharged from the slag-water mixture discharge pipe 5112 at low temperature, the safety risk of high-temperature slag discharge is reduced, and meanwhile, a large amount of diffusing gas is not generated after the low-temperature slag-water mixture is contacted with cooling water, thereby reducing the tail gas treatment pressure and reducing the environmental risk.
The permanent violet recycling device comprises a permanent violet slurrying kettle 521 and a permanent violet filter 522, wherein the permanent violet slurrying kettle 521 is connected with the slag discharging water tank 513, and the permanent violet filter 522 is connected with the permanent violet slurrying kettle 521. The permanent purple slurry kettle 521 is provided with a first o-dichlorobenzene feeding pipe 5211. And discharging the distillation residues into the permanent violet slurrying kettle 521, feeding an o-dichlorobenzene solvent into the permanent violet slurrying kettle 521 through the first o-dichlorobenzene feeding pipe 5211, pulping to fully dissolve the distillation residues and form permanent violet slurry. And discharging the permanent violet slurry into the permanent violet filter 522, and filtering to obtain a filter cake, namely coarse permanent violet. The crude permanent violet is sent to the o-dichlorobenzene washing centrifuge 100 for refining.
Practice shows that the distillation residues can be recovered by 50-65% of the permanent violet in the residues after one-time extraction, the permanent violet unit consumption is reduced, the recycling of wastes is realized, and meanwhile, the production amount of dangerous wastes is reduced by about 20%, and the cost for treating the dangerous wastes is reduced.
In an embodiment, a heating jacket 214 is disposed on the outer side of the steam still 210, and the heating jacket 214 is connected with a heat transfer oil feed pipe 2141 and a heat transfer oil discharge pipe 2142, so as to provide auxiliary heating for the steam still 210 by using heat transfer oil, maintain the stability of the temperature and the top temperature of the steam still 210, and ensure the normal operation of steam distillation.
In yet another embodiment, the water washing and filter pressing device 300 is provided with a filtrate discharging pipe 320, and the filtrate discharging pipe 320 is connected with a filtrate buffer tank 321. In the water washing filter pressing device 300, the main component in the filter pressing filtrate is triethylamine hydrochloride after washing with hot water, the filtrate is discharged into the filtrate buffer pool 321 through the filtrate discharging pipe 320, and triethylamine in the filtrate is recovered by adding alkali solution for neutralization.
In one embodiment, a method for refining permanent violet comprises the following steps:
washing o-dichlorobenzene: washing the crude product of the permanent violet subjected to removal of the o-dichlorobenzene by using the o-dichlorobenzene, and after the o-dichlorobenzene is washed, centrifugally drying to obtain the permanent violet subjected to primary washing.
Namely, after removing the crude product of the permanent violet of the o-dichlorobenzene, firstly, at a certain temperature, introducing a certain flow of the o-dichlorobenzene into the o-dichlorobenzene washing centrifuge 100 through the o-dichlorobenzene feeding distribution disc 110, washing the crude product of the permanent violet by using the o-dichlorobenzene, and removing substances dissolved in the crude product of the permanent violet, in particular substances such as nitro substances, benzenesulfonyl chloride, tetrachlorobenzoquinone, phenylthiol and the like. And (3) after the o-dichlorobenzene is washed, spin-drying is carried out by the o-dichlorobenzene washing centrifugal machine 100, the centrifugal mother liquor is collected and uniformly treated, and the centrifugal filter cake is the primary washing permanent violet, and the primary washing permanent violet at the moment contains a larger residual amount of o-dichlorobenzene component.
Steam distillation: pulping the primary washing permanent violet, introducing steam into a distillation kettle, and performing steam distillation to remove o-dichlorobenzene to obtain the secondary washing permanent violet.
Conventionally, the primary washing permanent violet is subjected to secondary washing with the nekal water to reduce the content of o-dichlorobenzene in the primary washing permanent violet. However, the o-dichlorobenzene is washed by the nekal water, on one hand, the residual quantity of the o-dichlorobenzene in the washing product is larger, the improvement of the product quality is limited, and on the other hand, the discharge amount of the waste water is large, and the washing waste water is introduced into sulfonate substances, so that the waste water treatment difficulty is larger.
Extracting residual o-dichlorobenzene in the permanent violet crude product by using a steam distillation mode, namely, delivering centrifugal filter residues obtained by washing the o-dichlorobenzene into a steam distillation device, heating water into a steam distillation kettle 210 through a hot water feeding pipe 211, and starting a beating stirrer 212 to perform beating. Steam is introduced into the steam distillation still 210 through the steam feed pipe 213, for example, steam with a temperature of 120-150 ℃ is introduced, on one hand, high temperature is provided to make o-dichlorobenzene contained in the centrifugal filter residue azeotropically distill with water, and on the other hand, due to the stripping action provided by the steam, o-dichlorobenzene is fully separated out of the centrifugal filter residue, so that the o-dichlorobenzene component in the centrifugal filter residue is effectively removed, and the residual of o-dichlorobenzene in the permanent violet is reduced.
Washing with hot water: filtering the secondary washing permanent violet by a filter press, washing a filter cake on the filter press by hot water, and filtering to obtain wet permanent violet.
That is, after the steam distillation is finished, the permanent violet slurry is sent to the water washing and filter-pressing device 300 for filter-pressing dehydration, and meanwhile, hot water is continuously heated to the water washing and filter-pressing device 300 through the hot water feeding distribution plate 310 for hot water washing, so as to remove the impurity components in the permanent violet, such as triethylamine hydrochloride, which are soluble in the hot water, and thus, a high-quality permanent violet finished product is obtained. Wherein the temperature of the hot water is 42-60 ℃.
After detection and three times of washing, the residual quantity of the o-dichlorobenzene in the permanent violet finished product is less than 500mg/kg and is far less than that of the traditional powder pulling washing (8000-10000 mg/kg of the o-dichlorobenzene in the traditional powder pulling washing), compared with the traditional process, the residual quantity of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanently fixed purple washing wastewater does not contain a powder pulling material, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is conveniently recovered from the wastewater, and the difficulty of wastewater treatment is reduced.
Drying and crushing: drying and crushing wet permanent violet to obtain refined permanent violet.
The foregoing disclosure is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the scope of the invention, as it is understood by those skilled in the art that all or part of the above-described embodiments may be practiced with equivalents thereof, which fall within the scope of the invention as defined by the appended claims.
Claims (7)
1. A system for refining a crude permanent violet product, comprising:
an ortho-dichlorobenzene washing centrifuge is provided with an ortho-dichlorobenzene feeding distribution disc; a centrifugal mother liquor discharging pipe is arranged on the o-dichlorobenzene washing centrifugal machine, a centrifugal mother liquor pool is connected on the centrifugal mother liquor discharging pipe,
the permanent violet crude product refining system further comprises a centrifugal mother liquor treatment unit, the centrifugal mother liquor treatment unit comprises an orthodichlorobenzene extraction device, the orthodichlorobenzene extraction device comprises a reduced pressure distillation kettle, an orthodichlorobenzene extraction component and a deslagging water tank, a centrifugal mother liquor feeding pipe is arranged on the reduced pressure distillation kettle, the centrifugal mother liquor feeding pipe is connected with an outlet end of a centrifugal mother liquor pond, a slag water mixture discharging pipe is arranged at the kettle bottom of the reduced pressure distillation kettle, the slag water mixture discharging pipe is connected with the deslagging water tank, the orthodichlorobenzene extraction device comprises a recovery condenser and a first condensate receiving tank, a hot side feeding end of the recovery condenser is connected with the reduced pressure distillation kettle, the first condensate receiving tank is connected with a condensate discharging end of the recovery condenser, a negative pressure generating piece is further connected with the first condensate receiving tank, a steam feeding pipe is further connected with the reduced pressure distillation kettle, the vacuum degree of the reduced pressure distillation kettle is controlled to be 40 KPa-60 KPa, the temperature of the distillation kettle is controlled to be 80-100 ℃, and the reduced pressure distillation is performed; after the reduced pressure distillation is finished, introducing steam with the temperature of 120-150 ℃ into the reduced pressure distillation kettle through the steam feed pipe, namely steam with the pressure of 0.2-0.5 MPa, and performing steam distillation;
the steam distillation device comprises a steam distillation kettle and an orthodichlorobenzene recycling component arranged at the top of the steam distillation kettle, wherein the feeding end of the steam distillation kettle is connected with the solid-phase discharging end of the orthodichlorobenzene washing centrifuge, and a hot water feeding pipe and a pulping stirrer are arranged on the steam distillation kettle; the kettle bottom of the water vapor distillation kettle is connected with a water vapor feeding pipe;
the feeding end of the water washing and pressure filtration device is connected with the discharging end of the tower kettle of the water vapor distillation kettle, and the water washing and pressure filtration device is provided with a hot water feeding distribution disc; and the post-treatment device comprises a filter cake dryer for drying the permanent violet filter cake from the washing filter-pressing device and a filter cake pulverizer for pulverizing the permanent violet filter cake.
2. The system of claim 1, wherein the orthodichlorobenzene recovery assembly comprises a condenser, an orthodichlorobenzene separator tank and a vacuum pump, wherein a hot material inlet section of the condenser is connected with a top gas phase discharge end of the water vapor distillation still, the orthodichlorobenzene separator tank is connected with a condensate discharge end of the condenser, and an inlet of the vacuum pump is connected with the orthodichlorobenzene separator tank.
3. The system for refining the crude permanent violet product according to claim 1, wherein a heating jacket is arranged on the outer side of the water vapor distillation kettle, and the heating jacket is connected with a heat conducting oil feeding pipe and a heat conducting oil discharging pipe.
4. The system for refining the crude permanent violet product according to claim 1, wherein a filtrate discharging pipe is arranged on the water washing and filter pressing device, and the filtrate discharging pipe is connected with a filtrate buffer pool.
5. The method for refining the permanent violet crude product is characterized by comprising the following steps of:
washing o-dichlorobenzene: washing the crude product of the permanent violet subjected to removal of the o-dichlorobenzene by using the o-dichlorobenzene, and after the o-dichlorobenzene is washed, centrifugally drying to obtain the permanent violet subjected to primary washing;
the permanent violet centrifugal mother liquor after centrifugation is subjected to reduced pressure distillation under the vacuum degree of 40 KPaA-60 KPaA and the temperature of 80 ℃ to 100 ℃, the evaporated gas phase is condensed and refluxed to be liquid phase for recycling, and after the reduced pressure distillation is finished, steam with the temperature of 120 ℃ to 150 ℃ is introduced into the distillation residue for steam distillation;
steam distillation: pulping the primary washing permanent violet, introducing steam into a distillation kettle, and performing steam distillation to remove o-dichlorobenzene to obtain secondary washing permanent violet;
washing with hot water: filtering the secondary washing permanent violet by a filter press, washing a filter cake on the filter press by hot water, and filtering to obtain wet permanent violet;
drying and crushing: drying and crushing wet permanent violet to obtain refined permanent violet.
6. The method for refining crude permanent violet according to claim 5, wherein in the step of steam distillation, steam with a temperature of 120-150 ℃ is introduced into a distillation still.
7. The method for refining a crude permanent violet product according to claim 5, wherein in the step of washing with hot water, the temperature of the hot water is 42 ℃ to 60 ℃.
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