CN111875977A - Permanent violet refining system and method - Google Patents
Permanent violet refining system and method Download PDFInfo
- Publication number
- CN111875977A CN111875977A CN202010879158.6A CN202010879158A CN111875977A CN 111875977 A CN111875977 A CN 111875977A CN 202010879158 A CN202010879158 A CN 202010879158A CN 111875977 A CN111875977 A CN 111875977A
- Authority
- CN
- China
- Prior art keywords
- dichlorobenzene
- permanent violet
- washing
- ortho
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 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 122
- 238000007670 refining Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 17
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims abstract description 280
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 106
- 238000005406 washing Methods 0.000 claims abstract description 96
- 238000004821 distillation Methods 0.000 claims abstract description 50
- 238000003825 pressing Methods 0.000 claims abstract description 22
- 238000004537 pulping Methods 0.000 claims abstract description 14
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 238000001256 steam distillation Methods 0.000 claims description 30
- 239000012065 filter cake Substances 0.000 claims description 24
- 239000012452 mother liquor Substances 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000011085 pressure filtration Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 15
- 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 6
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 abstract description 5
- 238000010533 azeotropic distillation Methods 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000008236 heating water Substances 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 9
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 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
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 5
- 235000011941 Tilia x europaea Nutrition 0.000 description 5
- 239000004571 lime Substances 0.000 description 5
- 239000000203 mixture Substances 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
- 238000000605 extraction Methods 0.000 description 4
- PLAZXGNBGZYJSA-UHFFFAOYSA-N 9-ethylcarbazole Chemical compound C1=CC=C2N(CC)C3=CC=CC=C3C2=C1 PLAZXGNBGZYJSA-UHFFFAOYSA-N 0.000 description 3
- 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
- 150000002828 nitro derivatives Chemical class 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 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
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000005125 dioxazines Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000000802 nitrating effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000013049 sediment Substances 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
- 239000002912 waste gas Substances 0.000 description 1
Images
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 permanent violet 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 filter pressing device and a post-treatment device, wherein the permanent violet crude product is firstly washed by o-dichlorobenzene in the o-dichlorobenzene washing centrifuge to remove substances dissolved in the o-dichlorobenzene in the permanent violet crude product. And (3) feeding the centrifugal filter residue into a water vapor distillation device, heating water for pulping, introducing steam, providing high temperature to ensure that the o-dichlorobenzene and the water in the centrifugal filter residue are subjected to azeotropic distillation on one hand, and providing a certain gas stripping effect to ensure that the o-dichlorobenzene is fully separated out from the centrifugal filter residue on the other hand, thereby reducing the residue of the o-dichlorobenzene in the permanent violet. And (3) sending the permanent violet slurry into a washing and filter-pressing device, performing filter-pressing dehydration, and simultaneously adding hot water for hot water washing to remove triethylamine hydrochloride. After three times of washing, the residual amount of the o-dichlorobenzene in the permanent violet finished product is obviously less 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 permanent violet refining method.
Background
The permanent violet RL is a high-grade organic pigment of dioxazine class, has outstanding tinting strength and brightness, excellent heat resistance and penetration 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, packaging printing and the like.
The permanent violet RL is produced by the following main processes: dissolving carbazole in alkali liquor for alkylation to obtain N-ethyl carbazole, nitrating N-ethyl carbazole in nitric acid, reducing N-ethyl carbazole in H2, condensing in tetrachlorobenzoquinone, ring-closing and oxidizing in benzenesulfonyl chloride to obtain permanent violet crude liquid, and filtering, drying and pulverizing to obtain the invented product. In the actual production, the permanent violet crude liquid is discharged at the temperature of 120 ℃, the solvent is removed by filtration, the filter cake is washed by o-dichlorobenzene, nekal water and hot water, and finally the finished product is prepared by filter pressing and drying.
The washing process for the permanent violet crude product has the following problems:
firstly, the residual quantity of o-dichlorobenzene is large, a large amount of waste gas is generated during plate and frame filter pressing and product drying, the environment is polluted, and safety risks exist.
Secondly, the washing wastewater discharge capacity is large due to the use of the pull-open powder as a detergent, the salt content and the COD value are increased, and the wastewater treatment difficulty is increased.
Disclosure of Invention
In view of the above, the invention provides a permanent violet refining system, which solves the technical problems of large residual quantity of o-dichlorobenzene, large wastewater discharge and difficult treatment in the crude permanent violet refining process in the prior art.
The invention also provides a refining method of the permanent violet.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a permanent violet refining system comprising:
an ortho-dichlorobenzene washing centrifugal machine, wherein an ortho-dichlorobenzene feeding distribution disc is arranged on the ortho-dichlorobenzene washing centrifugal machine;
the steam distillation device comprises a steam distillation kettle and an o-dichlorobenzene recovery assembly arranged at the top of the steam distillation kettle, wherein the feed end of the steam distillation kettle is connected with the solid-phase discharge end of the o-dichlorobenzene washing centrifugal machine, and the steam distillation kettle is provided with a hot water feed pipe and a pulping stirrer; the kettle bottom of the water vapor distillation kettle is connected with a water vapor feeding pipe;
the feeding end of the washing and filter-pressing device is connected with the discharging end of the tower kettle of the water vapor distillation kettle, and a hot water feeding distribution disc is arranged on the washing and filter-pressing device; and
and the post-treatment device comprises a filter cake dryer and a filter cake crusher, wherein the filter cake dryer is used for drying the permanent violet filter cake from the water washing and pressure filtering device, and the filter cake crusher is used for crushing the permanent violet filter cake.
Preferably, ortho-dichlorobenzene retrieves subassembly includes condenser, ortho-dichlorobenzene knockout drum and vacuum pump, the hot material import section of condenser is connected the gaseous discharge end in top of steam stills, ortho-dichlorobenzene knockout drum is connected the lime set discharge end of condenser, the entry connection of vacuum pump ortho-dichlorobenzene knockout drum.
Preferably, a centrifugal mother liquid discharging pipe is arranged on the o-dichlorobenzene washing centrifugal machine, and a centrifugal mother liquid pool is connected to the centrifugal mother liquid discharging pipe.
Preferably, the outer side of the water vapor distillation kettle is provided with a heating jacket, and the heating jacket is connected with a heat conduction oil feeding pipe and a heat conduction oil discharging pipe.
Preferably, a filtrate discharge pipe is arranged on the water washing and pressure filtering device and connected with a filtrate buffer pool.
A refining method of permanent violet comprises the following steps:
washing with o-dichlorobenzene: washing the crude product of the permanent violet after removal of the o-dichlorobenzene by using o-dichlorobenzene, and after washing of the o-dichlorobenzene is finished, centrifugally drying to obtain the once-washed permanent violet;
water vapor distillation: pulping the once-washed permanent violet, introducing steam into a distillation kettle, performing steam distillation, and removing o-dichlorobenzene to obtain a twice-washed permanent violet;
washing with hot water: filtering the secondarily washed permanent violet by a filter press, washing a filter cake on the filter press by hot water, and filtering to dryness to obtain wet permanent violet;
drying and crushing: the wet permanent violet is dried and crushed to obtain the 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 permanent violet refining method, which have the beneficial effects that: the o-dichlorobenzene washing centrifuge, the water vapor distillation device, the water washing and filter pressing device and the post-treatment device are sequentially arranged, and after the o-dichlorobenzene permanent violet crude product is removed, firstly, the o-dichlorobenzene is used for washing in the o-dichlorobenzene washing centrifuge at a certain temperature, so that substances dissolved in the o-dichlorobenzene in the permanent violet crude product, especially substances such as nitro compounds, benzenesulfonyl chloride, tetrachlorobenzoquinone, benzenethiol and the like, are removed. After washing of ortho-dichlorobenzene is finished, the ortho-dichlorobenzene is dried by the ortho-dichlorobenzene washing centrifugal machine, centrifugal mother liquor is collected and uniformly treated, centrifugal filter residues are fed into the water vapor distillation device, firstly, hot water is added for pulping, then steam is introduced, on one hand, high temperature is provided, so that the ortho-dichlorobenzene and the water contained in the centrifugal filter residues are subjected to azeotropic distillation, on the other hand, the steam provides a certain gas stripping effect, so that the ortho-dichlorobenzene is fully separated out of the centrifugal filter residues, ortho-dichlorobenzene components in the centrifugal filter residues are effectively removed, and residue of the ortho-dichlorobenzene in permanent violet is reduced. And after the water vapor distillation is finished, the permanent violet slurry is sent into the water washing and pressure filtering device for filter pressing and 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 three times of washing, the residual amount 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 washing (the residual amount of the o-dichlorobenzene in the traditional powder washing is 8000-10000 mg/kg), compared with the traditional process, the residual amount of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanent violet washing wastewater does not contain a nekal substance, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is convenient to recover 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, an ortho-dichlorobenzene washing centrifuge 100, an ortho-dichlorobenzene feeding distribution disc 110, a centrifugal mother liquid discharge pipe 120, a centrifugal mother liquid pool 130, a water vapor distillation kettle 210, a hot water feeding pipe 211, a pulping stirrer 212, a water vapor feeding pipe 213, a heating jacket 214, a heat conduction oil feeding pipe 2141, a heat conduction oil discharge pipe 2142, a condenser 221, an ortho-dichlorobenzene separation tank 222, a vacuum pump 223, a water washing and pressure filtering device 300, a hot water feeding distribution disc 310, a filtrate discharge pipe 320, a filtrate buffer pool 321, a filter cake dryer 410, a filter cake crusher 420, a reduced pressure distillation kettle 511, a centrifugal mother liquid feeding pipe 5111, a slag-water mixture discharge pipe 5112, a vapor feeding pipe 5113, a recovery condenser 5121, a first condensate receiving tank 5122, a negative pressure generating piece 5123, a residue discharging water pool 513, a permanent violet slurrying kettle 521, a permanent violet filter 522 and a first ortho-dichlorobenzene feeding pipe.
Detailed Description
The technical scheme and the technical effect of the invention are further elaborated in the following by combining the drawings of the invention.
Referring to fig. 1, in one embodiment, a permanent violet refining system 10 is provided for refining a permanent violet crude product. The method comprises the following steps: the device comprises an ortho-dichlorobenzene washing centrifugal machine 100, a water vapor distillation device, a water washing and filter pressing device 300 and a post-treatment device, wherein the ortho-dichlorobenzene washing centrifugal machine 100 is provided with an ortho-dichlorobenzene feeding distribution disc 110.
The steam distillation device comprises a steam distillation kettle 210 and an o-dichlorobenzene recovery assembly arranged at the top of the steam distillation kettle 210, wherein the feed end of the steam distillation kettle 210 is connected with the solid-phase discharge end of the o-dichlorobenzene washing centrifuge 100, and the steam distillation kettle 210 is provided with a hot water feed pipe 211 and a pulping stirrer 212. The bottom of the steam distillation still 210 is connected with a steam feeding pipe 213. The feed end of the water washing and filter pressing device 300 is connected with the tower kettle discharge 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-processing device comprises a filter cake dryer 410 for drying the permanent violet filter cake from the water washing and pressure filtering device 300 and a filter cake crusher 420 for crushing the permanent violet filter cake.
After the o-dichlorobenzene is removed, firstly, in the o-dichlorobenzene washing centrifuge 100, at a certain temperature, o-dichlorobenzene with a certain flow rate is introduced through the o-dichlorobenzene feeding distribution disc 110, and the o-dichlorobenzene is used for washing the crude o-dichlorobenzene to remove substances dissolved in the o-dichlorobenzene in the crude o-dichlorobenzene, especially substances such as nitro compounds, benzenesulfonyl chloride, tetrachlorobenzoquinone, benzenethiol and the like. After washing of o-dichlorobenzene is completed, the o-dichlorobenzene is dried by the o-dichlorobenzene washing centrifuge 100, centrifugal mother liquor is collected and uniformly treated, centrifugal filter residues are sent to the water vapor distillation device, firstly, water is added into the water vapor distillation kettle 210 through the hot water feeding pipe 211, and the pulping stirrer 212 is started for pulping. Steam is introduced into the water vapor distillation kettle 210 through the water vapor inlet pipe 213, for example, steam with the temperature of 120-150 ℃ is introduced, on one hand, high temperature is provided, so that o-dichlorobenzene and water contained in the centrifugal filter residue are subjected to azeotropic distillation, on the other hand, the o-dichlorobenzene is sufficiently separated out from the centrifugal filter residue under the gas stripping action provided by the steam, so that o-dichlorobenzene components in the centrifugal filter residue are effectively removed, and the residue of o-dichlorobenzene in permanent violet is reduced. After the water vapor distillation is finished, the permanent violet slurry is sent to the water washing and filter pressing device 300 for filter pressing and dehydration, and meanwhile, hot water is continuously added into the water washing and filter pressing device 300 through the hot water feeding distribution disc 310 for hot water washing so as to remove impurity components such as triethylamine hydrochloride in the permanent violet which can be dissolved in the hot water, and thus a high-quality permanent violet finished product is obtained.
After three times of washing, the residual amount 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 washing (the residual amount of the o-dichlorobenzene in the traditional powder washing is 8000-10000 mg/kg), compared with the traditional process, the residual amount of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanent violet washing wastewater does not contain a nekal substance, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is convenient to recover from the wastewater, and the difficulty of wastewater treatment is reduced.
In one embodiment, the ortho-dichlorobenzene recycling assembly comprises a condenser 221, an ortho-dichlorobenzene separation 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 steam distillation still 210, the ortho-dichlorobenzene separation 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 ortho-dichlorobenzene separation tank 222. Under the action of the vacuum pump 223, the pressure at the top of the water vapor distillation kettle 210 is maintained to be 40 KPaA-60 KPaA (KPaA represents absolute pressure unit), water and o-dichlorobenzene are azeotroped, a gas phase passes through the bottom of the water vapor distillation kettle 210 and enters the condenser 221 for condensation, a condensate automatically flows into the o-dichlorobenzene separation tank 222, water and o-dichlorobenzene are layered, and o-dichlorobenzene is recovered.
In another embodiment, the ortho-dichlorobenzene washing centrifuge 100 is provided with a centrifuge mother liquor discharge pipe 120, and a centrifuge mother liquor pool 130 is connected to the centrifuge mother liquor discharge pipe 120. The centrifugal mother liquor containing a large amount of o-dichlorobenzene centrifugally separated by the o-dichlorobenzene washing centrifuge 100 enters the centrifugal mother liquor pool 130 through the centrifugal mother liquor discharge pipe 120, and is collected and treated in a centralized manner to recover the o-dichlorobenzene component in the centrifugal mother liquor.
In an embodiment, the permanent violet refining system 10 further includes a centrifugal mother liquor processing unit, and the centrifugal mother liquor processing unit includes an ortho-dichlorobenzene extraction device and a permanent violet recovery device.
Ortho-dichlorobenzene extraction element includes vacuum distillation cauldron 511, ortho-dichlorobenzene extraction element and row sediment pond 513, be provided with centrifugal mother liquor inlet pipe 5111 on the vacuum distillation cauldron 511, centrifugal mother liquor inlet pipe 5111 is connected the exit end in 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 discharging water tank 513. Ortho-dichlorobenzene draws subassembly receives groove 5122 including retrieving condenser 5121 and first lime set, the hot side feed end of retrieving condenser 5121 is connected reduced pressure stills 511, first lime set receives the groove 5122 to be connected retrieve condenser 5121's lime set discharge end, still be connected with negative pressure generation piece 5123 on the first lime set receives the groove 5122. The vacuum still 511 is also connected to 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 feeding pipe 5111, and is firstly subjected to reduced pressure distillation. Controlling the vacuum degree of the distillation kettle to be 40 KPaA-60 KPaA (KPaA represents absolute pressure unit), and the temperature of the distillation kettle to be 80-100 ℃ to carry out reduced pressure distillation. The ortho-dichlorobenzene component in the permanent violet centrifugal mother liquor is evaporated, and after an evaporated gas phase is condensed by the recovery condenser 5121, the ortho-dichlorobenzene with the mass concentration of 70-80% is mainly contained in the condensate, and the condensate is collected in the first condensate receiving tank 5122 for recycling. Other components (mainly comprising about 35% of permanent violet, about 25% of benzenesulfonic acid triethylamine salt 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. When most of o-dichlorobenzene was distilled out of the system, the remaining components were present in the form of distillation residue in the vacuum distillation still 511.
After the reduced pressure distillation is finished, the distillation residue mainly contains permanent violet, benzenesulfonic acid triethylamine salt, tetrachlorobenzoquinone and a small amount of o-dichlorobenzene components, and steam (namely, steam with the pressure of 0.2MPa to 0.5 MPa) with the temperature of 120 ℃ to 150 ℃ is introduced into the reduced pressure distillation kettle 511 through the steam inlet pipe 5113 for steam distillation. In the distillation process, an azeotropic system of steam and o-dichlorobenzene is formed, the steam is assisted to be stripped by steam, the steam carrying the o-dichlorobenzene steam is discharged from the gas phase of the reduced pressure distillation kettle 511 and condensed by the recovery condenser 5121, the condensate mainly contains water and o-dichlorobenzene and is collected in the first condensate receiving groove 5122, and the o-dichlorobenzene is recycled after oil-water separation. Meanwhile, steam is condensed, salts (such as triethylamine benzenesulfonate) contained in distillation residues are dissolved in 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 residue-water mixture discharge pipe 5112 at a low temperature, the safety risk of high-temperature slag discharge is reduced, and simultaneously, a large amount of diffused gas cannot be generated after the low-temperature residue-water mixture is contacted with cooling water, so that the tail gas treatment pressure is reduced, and the environmental risk is reduced.
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. A first ortho-dichlorobenzene feed pipe 5211 is arranged on the permanent violet slurry kettle 521. 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, and pulping to fully dissolve the distillation residues to form permanent violet slurry. And discharging the permanent violet slurry into the permanent violet filter 522, and filtering to obtain a filter cake, namely the coarse permanent violet. The crude permanent violet is fed to the o-dichlorobenzene washing centrifuge 100 for refining.
Practice shows that distillation residues can recover 50% -65% of the permanent violet in the residues after one-time extraction, the unit consumption of the permanent violet is reduced, the recycling of wastes is realized, meanwhile, the generation 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 outside the steam distillation still 210, and the heating jacket 214 is connected to a heat conduction oil feeding pipe 2141 and a heat conduction oil discharging pipe 2142, so as to provide auxiliary heating for the steam distillation still 210 by using heat conduction oil, maintain the stability of the still temperature and the top temperature of the steam distillation still 210, and ensure the normal operation of steam distillation.
In another embodiment, the water washing pressure filter device 300 is provided with a filtrate outlet pipe 320, and the filtrate outlet pipe 320 is connected with a filtrate buffer pool 321. In the water washing and filter-pressing device 300, hot water washing is performed, the main component in filter-pressing filtrate is triethylamine hydrochloride, the filtrate is discharged into the filtrate buffer pool 321 through the filtrate discharge pipe 320, and triethylamine in the filtrate is recovered through neutralization by adding alkaline solution.
In a specific embodiment, a refining method of permanent violet comprises the following steps:
washing with o-dichlorobenzene: washing the crude product of the permanent violet after removing the o-dichlorobenzene by using o-dichlorobenzene, and centrifugally drying after the washing of the o-dichlorobenzene is finished to obtain the once-washed permanent violet.
Namely, after removing the ortho-dichlorobenzene, firstly, in the ortho-dichlorobenzene washing centrifuge 100, at a certain temperature, a certain flow of ortho-dichlorobenzene is introduced through the ortho-dichlorobenzene feeding distribution disc 110, and the ortho-dichlorobenzene is used for washing the crude product of the ortho-dichlorobenzene, so as to remove substances dissolved in the ortho-dichlorobenzene in the crude product of the ortho-dichlorobenzene, especially substances such as nitro compounds, benzenesulfonyl chloride, tetrachlorobenzoquinone, benzenethiol and the like. And after the washing of the o-dichlorobenzene is finished, the o-dichlorobenzene is dried by the o-dichlorobenzene washing centrifugal machine 100, centrifugal mother liquor is collected and uniformly treated, a centrifugal filter cake is once-washing permanent violet, and the once-washing permanent violet contains a large residual amount of the o-dichlorobenzene component.
Water vapor distillation: pulping the once-washed permanent violet, introducing steam into a distillation kettle, performing steam distillation, and removing o-dichlorobenzene to obtain the twice-washed permanent violet.
Traditionally, the once-washed permanent violet is washed twice with nekal water to reduce the content of o-dichlorobenzene in the once-washed permanent violet. However, when the o-dichlorobenzene is washed by the undrawn powder water, on one hand, the residual amount of the o-dichlorobenzene in a washing product is large, so that the improvement of the product quality is limited, and on the other hand, the discharge amount of wastewater is large, and the difficulty in wastewater treatment is large due to the introduction of sulfonate substances into the washing wastewater.
Residual o-dichlorobenzene in the permanent violet crude product is extracted by means of steam distillation, namely centrifugal filter residue obtained by washing the o-dichlorobenzene is fed into the steam distillation device, water is firstly added into the steam distillation kettle 210 through the hot water feeding pipe 211, and the pulping stirrer 212 is started for pulping. Steam is introduced into the water vapor distillation kettle 210 through the water vapor inlet pipe 213, for example, steam with the temperature of 120-150 ℃ is introduced, on one hand, high temperature is provided, so that o-dichlorobenzene and water contained in the centrifugal filter residue are subjected to azeotropic distillation, on the other hand, the o-dichlorobenzene is sufficiently separated out from the centrifugal filter residue under the gas stripping action provided by the steam, so that o-dichlorobenzene components in the centrifugal filter residue are effectively removed, and the residue of o-dichlorobenzene in permanent violet is reduced.
Washing with hot water: and filtering the twice-washed permanent violet by using a filter press, washing a filter cake on the filter press by using hot water, and filtering to dryness to obtain the wet permanent violet.
That is to say, after the water vapor distillation is finished, the permanent violet slurry is sent to the water washing and filter pressing device 300 for filter pressing and dehydration, and meanwhile, hot water is continuously added into the water washing and filter pressing device 300 through the hot water feeding distribution disc 310 for hot water washing, so that impurity components which can be dissolved in hot water, such as triethylamine hydrochloride in the permanent violet, are removed, and a high-quality permanent violet finished product is obtained. Wherein the temperature of the hot water is 42-60 ℃.
After three times of washing, the residual amount 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 washing (the residual amount of the o-dichlorobenzene in the traditional powder washing is 8000-10000 mg/kg), compared with the traditional process, the residual amount of the o-dichlorobenzene is greatly reduced, and the quality of the permanent violet finished product is improved. Meanwhile, the permanent violet washing wastewater does not contain a nekal substance, so that the discharge capacity of the wastewater is reduced, the triethylamine salt component is convenient to recover from the wastewater, and the difficulty of wastewater treatment is reduced.
Drying and crushing: the wet permanent violet is dried and crushed to obtain the refined permanent violet.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A permanent violet refining system, comprising:
an ortho-dichlorobenzene washing centrifugal machine, wherein an ortho-dichlorobenzene feeding distribution disc is arranged on the ortho-dichlorobenzene washing centrifugal machine;
the steam distillation device comprises a steam distillation kettle and an o-dichlorobenzene recovery assembly arranged at the top of the steam distillation kettle, wherein the feed end of the steam distillation kettle is connected with the solid-phase discharge end of the o-dichlorobenzene washing centrifugal machine, and the steam distillation kettle is provided with a hot water feed pipe and a pulping stirrer; the kettle bottom of the water vapor distillation kettle is connected with a water vapor feeding pipe;
the feeding end of the washing and filter-pressing device is connected with the discharging end of the tower kettle of the water vapor distillation kettle, and a hot water feeding distribution disc is arranged on the washing and filter-pressing device; and
and the post-treatment device comprises a filter cake dryer and a filter cake crusher, wherein the filter cake dryer is used for drying the permanent violet filter cake from the water washing and pressure filtering device, and the filter cake crusher is used for crushing the permanent violet filter cake.
2. The permanent violet refining system of claim 1, wherein the ortho-dichlorobenzene recycling assembly comprises a condenser, an ortho-dichlorobenzene separation 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 steam still, the ortho-dichlorobenzene separation tank is connected with a condensate discharge end of the condenser, and an inlet of the vacuum pump is connected with the ortho-dichlorobenzene separation tank.
3. The permanent violet refining system of claim 1, wherein the ortho-dichlorobenzene washing centrifuge is provided with a centrifugal mother liquor discharge pipe, and a centrifugal mother liquor pool is connected to the centrifugal mother liquor discharge pipe.
4. The permanent violet refining system 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 conduction oil feeding pipe and a conduction oil discharging pipe.
5. The permanent violet refining system of claim 1, wherein a filtrate outlet pipe is arranged on the water washing pressure filtration device, and the filtrate outlet pipe is connected with a filtrate buffer pool.
6. The refining method of permanent violet is characterized by comprising the following steps:
washing with o-dichlorobenzene: washing the crude product of the permanent violet after removal of the o-dichlorobenzene by using o-dichlorobenzene, and after washing of the o-dichlorobenzene is finished, centrifugally drying to obtain the once-washed permanent violet;
water vapor distillation: pulping the once-washed permanent violet, introducing steam into a distillation kettle, performing steam distillation, and removing o-dichlorobenzene to obtain a twice-washed permanent violet;
washing with hot water: filtering the secondarily washed permanent violet by a filter press, washing a filter cake on the filter press by hot water, and filtering to dryness to obtain wet permanent violet;
drying and crushing: the wet permanent violet is dried and crushed to obtain the refined permanent violet.
7. The method for refining permanent violet according to claim 6, wherein in the step of steam distillation, steam with the temperature of 120-150 ℃ is introduced into a distillation kettle.
8. The method of refining permanent violet according to claim 1, wherein the temperature of the hot water in the step of hot water washing is 42 ℃ to 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010879158.6A CN111875977B (en) | 2020-08-27 | 2020-08-27 | Permanent violet refining system and refining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010879158.6A CN111875977B (en) | 2020-08-27 | 2020-08-27 | Permanent violet refining system and refining method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111875977A true CN111875977A (en) | 2020-11-03 |
| CN111875977B CN111875977B (en) | 2023-10-31 |
Family
ID=73199860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010879158.6A Active CN111875977B (en) | 2020-08-27 | 2020-08-27 | Permanent violet refining system and refining method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111875977B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4345074A (en) * | 1980-03-21 | 1982-08-17 | Cassella Aktiengesellschaft | Process for the manufacture of a violet organic pigment, C.I. Pigment Violet 23 |
| WO2012001708A1 (en) * | 2010-06-30 | 2012-01-05 | Gharda Keki Hormusji | Process for preparing of dioxazine pigments |
| CN104031400A (en) * | 2014-06-25 | 2014-09-10 | 南通海迪化工有限公司 | Preparation method of permanent violet pigment |
| JP2018016742A (en) * | 2016-07-28 | 2018-02-01 | Dic株式会社 | Method for refining organic pigment |
| CN107814723A (en) * | 2017-11-14 | 2018-03-20 | 南通龙翔新材料科技股份有限公司 | The recovery method of triethylamine in a kind of permanent violet preparation process |
| CN108285189A (en) * | 2018-04-11 | 2018-07-17 | 银川百泓新材料科技有限公司 | A kind of method of extraction by steam distillation o-dichlorohenzene |
| CN108580062A (en) * | 2018-04-23 | 2018-09-28 | 江苏大洋环保工程有限公司 | A kind of centrifugation drum unit |
| CN110591408A (en) * | 2019-09-26 | 2019-12-20 | 新疆博蓝科精细化工有限公司 | Washing process for permanent violet crude product |
| CN212293389U (en) * | 2020-08-27 | 2021-01-05 | 银川百泓新材料科技有限公司 | Permanent purple refining system |
-
2020
- 2020-08-27 CN CN202010879158.6A patent/CN111875977B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4345074A (en) * | 1980-03-21 | 1982-08-17 | Cassella Aktiengesellschaft | Process for the manufacture of a violet organic pigment, C.I. Pigment Violet 23 |
| WO2012001708A1 (en) * | 2010-06-30 | 2012-01-05 | Gharda Keki Hormusji | Process for preparing of dioxazine pigments |
| CN104031400A (en) * | 2014-06-25 | 2014-09-10 | 南通海迪化工有限公司 | Preparation method of permanent violet pigment |
| JP2018016742A (en) * | 2016-07-28 | 2018-02-01 | Dic株式会社 | Method for refining organic pigment |
| CN107814723A (en) * | 2017-11-14 | 2018-03-20 | 南通龙翔新材料科技股份有限公司 | The recovery method of triethylamine in a kind of permanent violet preparation process |
| CN108285189A (en) * | 2018-04-11 | 2018-07-17 | 银川百泓新材料科技有限公司 | A kind of method of extraction by steam distillation o-dichlorohenzene |
| CN108580062A (en) * | 2018-04-23 | 2018-09-28 | 江苏大洋环保工程有限公司 | A kind of centrifugation drum unit |
| CN110591408A (en) * | 2019-09-26 | 2019-12-20 | 新疆博蓝科精细化工有限公司 | Washing process for permanent violet crude product |
| CN212293389U (en) * | 2020-08-27 | 2021-01-05 | 银川百泓新材料科技有限公司 | Permanent purple refining system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111875977B (en) | 2023-10-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1079008A (en) | Solvent pulping process | |
| US4496426A (en) | Process for the continuous extraction of vegetable-fiber material in two stages | |
| CN101302187B (en) | Production process of carbazol and anthracene | |
| CN212293389U (en) | Permanent purple refining system | |
| CN111362231B (en) | System and method for extracting sulfur from sulfur-containing foam of coking plant | |
| CN113443977A (en) | Sulfur and chlorine removal process in 2-ethyl anthraquinone production | |
| CN212293390U (en) | Permanent purple centrifugal mother liquor processing system | |
| CN108314637A (en) | A kind of preparation method and process units of thioacetic acid | |
| CN111875977B (en) | Permanent violet refining system and refining method | |
| CN103979577B (en) | A kind of coking desulfurization mixed salt extracts the method for sodium sulfocyanate | |
| WO2013018959A1 (en) | Method for manufacturing clean fuel, and reactor for extracting and separating organic components therefor | |
| CN116180480A (en) | Efficient methods and compositions for recovery of products from organic acid pretreatment of plant material | |
| CN212864621U (en) | Permanent purple centrifugal mother liquor recycling treatment system | |
| CN110423236B (en) | Preparation method of fluorescent whitening agent for whitening textiles | |
| CN104624616B (en) | A kind of indigo production mixes its Future about Alkaline Residue Treatment Unit and processing method | |
| CN111849192A (en) | Permanent purple centrifugal mother liquor processing system | |
| CN212864628U (en) | System for recovering permanent violet from permanent violet centrifugal mother liquor | |
| CN212864612U (en) | Recovery system of triethylamine for permanent violet production | |
| CN212864627U (en) | Permanent purple crude washing system | |
| CN212864605U (en) | Device for recovering o-dichlorobenzene from permanent violet centrifugal mother liquor | |
| CN212864629U (en) | Low-o-dichlorobenzene-residual permanent violet refining system | |
| CN111848338B (en) | Method and device for recovering o-dichlorobenzene from permanent violet centrifugal mother liquor | |
| CN110128283B (en) | 3, 5-diaminobenzoic acid production system and process | |
| CN212864614U (en) | Carbazole alkylation system | |
| CN105753744B (en) | A kind of H acid preparation facilities with energy-saving effect |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |