CS256581B1 - Method of waste waters cleaning from n-phenyl-n-isopropyl-p-phenylendiamine production - Google Patents
Method of waste waters cleaning from n-phenyl-n-isopropyl-p-phenylendiamine production Download PDFInfo
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- CS256581B1 CS256581B1 CS867189A CS718986A CS256581B1 CS 256581 B1 CS256581 B1 CS 256581B1 CS 867189 A CS867189 A CS 867189A CS 718986 A CS718986 A CS 718986A CS 256581 B1 CS256581 B1 CS 256581B1
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- waste water
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- toluene
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- aminodiphenylamine
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- 239000002351 wastewater Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000004140 cleaning Methods 0.000 title claims description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 46
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000126 substance Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract 2
- ATGUVEKSASEFFO-UHFFFAOYSA-N p-aminodiphenylamine Chemical compound C1=CC(N)=CC=C1NC1=CC=CC=C1 ATGUVEKSASEFFO-UHFFFAOYSA-N 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000005276 aerator Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004065 wastewater treatment Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000010802 sludge Substances 0.000 claims description 5
- 238000005273 aeration Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 230000002035 prolonged effect Effects 0.000 claims description 2
- 239000010865 sewage Substances 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 230000004907 flux Effects 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 235000013580 sausages Nutrition 0.000 claims 1
- PIOSEDPFJPAJKQ-UHFFFAOYSA-M sodium;toluene;hydroxide Chemical compound [OH-].[Na+].CC1=CC=CC=C1 PIOSEDPFJPAJKQ-UHFFFAOYSA-M 0.000 claims 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 150000002832 nitroso derivatives Chemical class 0.000 description 1
- OIJHFHYPXWSVPF-UHFFFAOYSA-N para-Nitrosodiphenylamine Chemical compound C1=CC(N=O)=CC=C1NC1=CC=CC=C1 OIJHFHYPXWSVPF-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000563 toxic property Toxicity 0.000 description 1
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- Removal Of Specific Substances (AREA)
- Physical Water Treatments (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
Riešenie sa týká spůsobu čistenia odpadových vůd z výroby N-fenyl-N‘-izopropyl-p- -fenyléndiamínu. Na odpadové vody s obsahom do 1,0 % hmot metanolu, připadne zriedené vodou až do objemového poměru 1 : 1, sa působí aromatickým uhlovodlkom so 6 až 8 atómami uhlíka, s výhodou toluénom, množstve 0,5 až 10,0 % hmot., vzhfadom na neriedené odpadové vody, pri teplote 35 až 110 °C a pri strednej době zdržania 0,5 až 60 minút. Riešenie je možné využit v chemickom priemysle.The solution relates to the method of waste treatment leader of N-phenyl-N‘-isopropyl-p- phenylenediamine. For waste water with content to 1.0% by weight of methanol, optionally diluted with water to volume ratio 1: 1, is treated with an aromatic hydrocarbon C 6 -C 8, preferably toluene, 0.5 to 10.0% by weight, with regard to untreated waste water, at at a temperature of 35 to 110 ° C and at medium time delay of 0.5 to 60 minutes. The solution is possible used in the chemical industry.
Description
Vynález sa týká sposobu čistenia odpadových vod z výroby N-fenyl-N‘-izopropyl-p-fenyléndiamínu.The present invention relates to a process for the purification of waste water from the production of N-phenyl-N‘-isopropyl-p-phenylenediamine.
Pri výrobě antiozonantu N-fenyl-N‘-izopropyl-p-fenyléndiamínu sa používá ako' medziprodukt 4-amínodifenyl-amín, připravený katalytickou redukciou vodno-metanolického roztoku sodnej soli 4-nitrózodifenylamínu vodíkom za přítomnosti organického rozpúšfadla a s použitím kovových hydrogenačných katalyzátorov (ČS AO 184 062). Vzniknutá emulzia vodnej a organickej fázy sa v separátore rozdělí a vodná fáza s obsahom 15 až 20 % metanolu sa vedie do kolony na regeneráciu metanolu. Organická fáza s obsahom 4-amínodifenylamínu sa vedie na rektifikačné kolony, kde sa v troch stupňoch izoluje čistý 4-amínodifenylamín, ktorý sa používá v ďalšom syntéznom stupni. Vařákový zvyšok v metanolovej koloně tvoria farebné odpadové vody s obsahom metanolu do 1,0 %. Sfarbenie je spósobené obsahom 4-amínodifenylamínu, nitro- a nitrózoderivátmi difenylamínu [do 0,5 % hmot.). Odpadové vody ďalej obsahujú 2 až 10 % hmot. NaOH a 5 až 10 % NaCl. Chemická spotřeba kyslíka (CHSK) pri týchto odpadových vodách je 30 000 až 60 000 mg O2/I.In the preparation of the N-phenyl-N'-isopropyl-p-phenylenediamine antiozonant, 4-aminodiphenylamine is prepared as an intermediate prepared by catalytic reduction of an aqueous methanolic solution of 4-nitrosodiphenylamine sodium with hydrogen in the presence of an organic solvent and using metal hydrogenation catalysts. AO 184 062). The resulting aqueous and organic phase emulsions are separated in a separator and the aqueous phase containing 15-20% methanol is fed to a methanol recovery column. The organic phase containing 4-aminodiphenylamine is fed to rectification columns, where pure 4-aminodiphenylamine is isolated in three steps, which is used in the next synthesis step. The residue in the methanol column consists of colored waste water with a methanol content of up to 1.0%. The coloring is due to the content of 4-aminodiphenylamine, nitro- and nitroso derivatives of diphenylamine [up to 0.5% by weight]. The waste water further comprises 2 to 10 wt. NaOH and 5 to 10% NaCl. The chemical oxygen demand (COD) for these waste waters is 30,000 to 60,000 mg O2 / L.
Odpadové vody s teplotou 105 až 115 °C sa cez utilizátor tepla, kde sa ochladla na teplotu 40 až 60 °C, vedu na chemická úpravu, ktorá spočívá v neutralizácii minerélnou kyselinou a v separácii chemického kalu, vylúčeného pri neutralizácii.The waste water at 105-115 ° C is passed through a heat utilizer, where it has been cooled to 40-60 ° C, to undergo a chemical treatment consisting of neutralization with mineral acid and separation of the chemical sludge that is eliminated during neutralization.
Manipulácia s odpadovými vodami a ich transport na chemická úpravu sú v podstatnej miere negativno ovplyvňované vylučováním časti organických látok, tvoriacich postupné smolovité usadeniny na stěnách zásobníkov, potrubia a armatúr a to až do takej miery, že dochádza k ich zaneseniu, čo si vyžaduje odstavenie technologického procesu. Takto zanesené technologické zariadenie sa musí čistil manuálně, pričom dochádza k styku s nebezpečnými a zdraviu škodlivými látkami.Wastewater handling and transport for chemical treatment is substantially negatively influenced by the elimination of a part of organic substances forming gradual pitch deposits on the walls of tanks, pipelines and fittings to the extent that they become clogged, which requires the shutdown of the technological process. process. The process equipment so clogged must be cleaned manually, in contact with hazardous and harmful substances.
Likvidácia polotuhých organických látok je problematická, pretože deponácia na skládku tuhého odpadu nie je možná vzhladom na ich toxické vlastnosti. Spalovanie si vyžaduje zasa speciálně zariadenie. Vysoká CHSK odpadových vód si vyžaduje poměrně nákladná chemickú úpravu před odvodom na biologické čistenie. Je preto žiadúce v odpadových vodách znížif obsah organických látok a následné CHSK už před ich vstupom na chemickú úpravu.The disposal of semi-solid organic substances is problematic, since deposition in a solid waste dump is not possible due to their toxic properties. Incineration requires a special device. The high COD of waste water requires a relatively expensive chemical treatment prior to removal for biological treatment. It is therefore desirable to reduce the content of organic substances in wastewater and the subsequent COD before they enter the chemical treatment.
V praxi sa zistilo, že biologické čistenie týchto odpadových vód s obsahom 4-amínodifenylamínu je skomplikované tvorbou pěny v aerátoroch, čo znižuje účinnosl procesu biologického čistenia a vyžaduje si následná aplikáciu odpeňovacích prostriedkov.In practice, it has been found that the biological purification of these 4-aminodiphenylamine-containing waste waters is complicated by the formation of foam in the aerators, which reduces the efficiency of the biological purification process and requires subsequent application of antifoams.
Z obsahu 4-amínodifenylamínu v odpadových vodách (0,05 až 0,2 % hmot.) vyplývá, že doteraz sa takto stráca bez užitku 0,5 až 1,0 % hmot. z celkového množstva 4-amínodifenylamínu v technologickom procese výroby N-fenyl-N‘-izopropyl-p-fenyléndiamínu a jeho recykláž do procesu je vzhladom na vysoká cenu, žiadúca aj z ekonomického hladiska.The content of 4-aminodiphenylamine in the waste water (0.05 to 0.2% by weight) shows that up to now, 0.5 to 1.0% by weight has been lost. of the total amount of 4-aminodiphenylamine in the technological process of producing N-phenyl-N‘-isopropyl-p-phenylenediamine and its recycling to the process is due to the high cost, also desirable from an economic point of view.
Uvedené nedostatky odstraňuje spósob čistenia týchto odpadových vód podlá vynálezu, ktorého podstata spočívá v tom, že na odpadové vody s obsahom metanolu do 1,0 % hmot., připadne zriedené vodou až do objemového poměru 1 : 1 sa pósobí aromatickým uhlovodíkom, s výhodou toluenem, benzénom, xylénom alebo ich zmesou v množstve 0,5 až 10 % hmot. vzhladom na neriedené odpadové vody, pri teplote 35 až 110 °C a pri strednej době zdržania 0,5 až 60 minút.The above-mentioned drawbacks are eliminated by the method of purification of these waste waters according to the invention, which consists in the treatment of waste waters with a methanol content of up to 1.0% by weight, optionally diluted with water up to a volume ratio of 1: 1. %, benzene, xylene or a mixture thereof in an amount of 0.5 to 10 wt. with respect to undiluted waste water at a temperature of 35 to 110 ° C and a mean residence time of 0.5 to 60 minutes.
Čistěním odpadových vód podlá vynálezu sa z odpadových vód 4-amínodifenylamín odstráni takmer úplné. Odstránia sa i časť vysokomolekulárnych látok, ktoré spolu s 4-amínodifenylamínom spósobujú vysokú CHSK odpadových vód a penenie v aerátoroch pri ich čistění na biologickej čistiarni, resp. po ochladení sa postupné vylučujú, s čím sú spojené už spomenuté problémy.Purification of the waste waters of the invention removes almost 4-aminodiphenylamine from the waste waters. Some of the high molecular weight substances that together with 4-aminodiphenylamine cause high COD of waste water and foaming in aerators during their purification at the biological treatment plant, respectively, are removed. after cooling, they are gradually eliminated, with which the aforementioned problems are associated.
Čistenie odpadových vód podlá vynálezu je možné robit bud rozmiešaním obidvoch fáz a ich následnou separáciou, alebo v zariadení s účinnosťou niekolkých teoretických stupňoch. Potřebná úroveň čistenia závisí od obsahu znečisťujúcich látok a je možné ju meniť aj množstvom použitého rozpúšťadla.The wastewater treatment according to the invention can be carried out either by mixing the two phases and then separating them, or in a plant with efficiency of several theoretical stages. The level of cleaning required depends on the pollutant content and can also be varied by the amount of solvent used.
Aromatické uhlovodíky sú na čistnie odpadových vód podlá vynálezu optimálně, v odpadových vodách s obsahom soli do 20 % sú prakticky nerozpustné, majú pro separáciu 4-amínodifenylamínu a jiných derivátov difenylamínov vysoký rozdělovači koeficient a sú poměrně lačné. Najvýhodnejšie sú toluén, benzen, xylen a ich zmesi.Aromatic hydrocarbons are optimal for wastewater treatment according to the invention, are practically insoluble in wastewater with a salt content of up to 20%, have a high partition coefficient for separation of 4-aminodiphenylamine and other diphenylamine derivatives and are relatively fasting. Most preferred are toluene, benzene, xylene and mixtures thereof.
Výhodou nášho postupu je, že sa prakticky kvantitativné odstráni vylučovanie organických látok, ktoré majú sklon tvořit smolovité usadeniny z odpadových vód po oddestilovaní metanolu a po ich ochladení. Odstráni sa tak zanášanie potrubných trás a aparátov a s tým spojené odstávky technologického procesu a s negativným dopadem na produkciu a ekonomiku procesu. Odpadá nutnost častého čistenia technologického zariadenia spojená s manipuláciou so smolovitými polotuhými zdraviu škodlivými látkami.The advantage of our process is that the excretion of organic substances, which tend to form pitch deposits from waste water after the methanol has been distilled off and cooled, is virtually quantitatively removed. This will eliminate fouling of pipelines and apparatuses and the associated downtime of the technological process and the negative impact on the production and economy of the process. There is no need for frequent cleaning of the technological equipment associated with the handling of pitch semi-solid substances harmful to health.
Tieto látky (prevažne sa jedná o- 4-amínodifenylamín) sa postupom podlá vynálezu izolujú z odpadových vód vo formě roztoku v organickom rozpúšťadle, ktorý sa recykluje do technologického procesu, kde sa spracuje v příslušném zariadení a takto sa 0,5 až 1 % 4-amínodifenylamínu (z celkového množstva 4-amínodifenylamínu vyrobeného katalytickou redukciou v predchá25B dazjúcom stupni) vracia znova do výroby N-fenyl-N‘-izopropyl-p-fenyléndiamínu. Prítomnosť sprievodných látok v recyklovanom roztoku nie je na závadu, pretože 4 -amínodifenylamín sa v technologickom procese čistí trojstupňovou rektifikáciou a látky sprevádzajúce recyklovaný 4-amínodifenylamín sa podlá svojho charakteru rozdelia medzi predné rektifikačné frakcie a vařákové zvyšky.These substances (predominantly 4-aminodiphenylamine) are isolated by the process according to the invention from waste water in the form of a solution in an organic solvent, which is recycled to the technological process, where it is treated in the respective plant and thus 0.5 to 1%. -amino-diphenylamine (from the total amount of 4-amino-diphenylamine produced by catalytic reduction in the previous 25B stage) returns to the production of N-phenyl-N'-isopropyl-p-phenylenediamine. The presence of the accompanying substances in the recycled solution is not a problem, since the 4-aminodiphenylamine is purified in the process by a three-stage rectification process and the substances accompanying the recycled 4-aminodiphenylamine, according to their nature, are divided between the front rectification fractions and reboiler residues.
Ďalšou výhodou je zníženie CHSK odpadových vod, čo je z hladiska ich spracovania na biologickej čistiarni velmi žiadúce ako aj odstránenie niektorých látok (predovšetkým 4-amínodifenylamínu), ktoré ako prax ukázala sposobujú penenie odpadových vod v aerátoroch pri ich čistění na biologickej čistiarni odpadových vod.Another advantage is the reduction of COD wastewater, which is highly desirable from the point of view of treatment at a biological wastewater treatment plant, as well as the removal of some substances (especially 4-aminodiphenylamine) which have shown to cause foaming of wastewater in aerators.
Vynález je bližšie objasněný na konkrét nych príkladoch.The invention is illustrated by the following examples.
Příklad 1Example 1
500 ml odpadových vůd (CHSK,.,- 35 400 miligramov na liter) s obsahom metanolu 0,1 °/o hmot. s teplotou 110 °C bolo nahatých do banky a po ich ochladení na laboratórnu teplotu (počas 12 h) bolo zistené, že na dne a stranách banky sa vytvořili smolovité usadeniny rozpustné v zmesi toluén a hydroxid sodný (v pomere 1:1). Množstvo usadenín bolo cca 0,5 g/1 odpa dových vůd. CHSKcr odpadovéj vody bola stále vysoká — 34 600 mg/1. Odpadová vo da bola zneutralizovaná 31 % kyselinou chlorovodíkovou na pH — 6,5 a bol oddělený vylúčený kal v množstve 1,4 g/1.500 ml waste lines (COD, - 35 400 milligrams per liter) with a methanol content of 0.1% by weight. at 110 ° C was poured into a flask and after cooling to room temperature (over 12 h), it was found that pitch and pellets soluble in toluene / sodium hydroxide (1: 1 ratio) formed on the bottom and sides of the flask. The amount of sediment was about 0.5 g / l of waste leads. COD cr waste water was still high - 34 600 mg / 1st The waste water was neutralized with 31% hydrochloric acid to pH = 6.5 and the separated sludge was collected at 1.4 g / l.
Tieto odpadové vody boli nastrekované do modelu aerátora čistiarne odpadových vůd a pri různých úrovniach aerácie boio zistené, že dochádza k ich silnému peneniu.These waste waters were injected into the aerator model of the wastewater treatment plant, and at various levels of boio aeration it was found that their foaming was severe.
Příklad 2Example 2
K 1000 ml odpadových vod (CHSK,,,. ~= 35 420 mg/1) s obsahom metanolu 0,1 c;b hmot. s teplotou 110 °C sa přidalo 40 ml to luénu a emulzia sa v banke intenzívně pre81To 1000 ml of waste water (COD, = 35 420 mg / l) with a methanol content of 0.1 c ; at 110 [deg.] C. 40 ml of toluene were added and the emulsion was vigorously pre81 in the flask
m.iešala počas 50 minút. V oddelenej toluénovej fáze bola stanovené sušina (4,55 % hmot.). V sušině bolo stanovené 95 % 4-amínodifenylamínu, zvyšok bol tvořený derivátmi difenylaminů. Filtráciou odpadovej vody cez fritu S 4 po 48 h státia pri jej posíupnom ochladnutí na laboratórnu teplotu neboli zistené vylúčené nerozpustné látky. Ani pri dlhšom státí počas 100 h nedochádzalo k vylučovaniu nerozpustných látok. Chemická spotřeba kyslíka odpadovej vody po extrakcii toluénom bola CHSKcr = --= 26 620 mg/1.m. stirred for 50 minutes. In the separate toluene phase, the dry weight (4.55% by weight) was determined. In the dry matter, 95% of 4-aminodiphenylamine was determined, the remainder being diphenylamine derivatives. Filtration of the waste water through the frit S 4 for 48 hours at its gradual cooling to room temperature did not reveal any insoluble matter. Even after prolonged standing for 100 h, no precipitation of insoluble matter occurred. The chemical oxygen demand of the waste water after toluene extraction was COD cr = - = 26 620 mg / l.
Příklad 3Example 3
Odpadové vody s chemickou spotřebou kyslíka CHSK., = 34 800 mg/1 s obsahom metanolu 0,1 % hmot. s teplotou 110 °C sa kontinuitne nastrekovalo do miešacej banky, kde sa přidávala voda v množstve 10 % hmot. na uvedené odpadové vody. Ďalej sa do banky privádzal toluén v množstve 2 % hmot. na uvedené odpadové vody. Zdržná doba emulzií v banke bola 2 minútv. V deliacom lieviku bola oddělená toluenová fáza, ktorá mala sušinu 9,6 % hmot. Analýzou sušiny bolo zistené, že je tvořená 95 % 4-amínodifenylamínu, zvyšok tvoria deriváty difenylaminů. Filtráciou odpadovej vody cez fritu S 4 po 48 h státia a po jej súčasnom ochladnutí na laboratórnu teplotu bolo zistené, že vylúčených nerozpustných látok bolo menej ako 0,1 mg/1. CHSKcr odpadovej vody po extrakcii toluénom bola 26 140 mg/i vzhladom na neriedené odpadové vody. Takto upravené odpadové vody boli zneutralizované 31 °/o kyselinou chlorovodíkovou na pH = 6,5 a bol oddělený vylúčený chemický kal v množstve 1,5 g/1. Tieto odpadové vody malí chemickú spotřebu kyslíka CHSKcr = 20 820 mg/1 a boli nastrekované do laboratórneho modelu aerátora čistiarne odpadových vod. Pri různých úrovniach aerácie bolo zistené, že pri spracovaní takto upravených odpadových vůd penenie bolo výrazné potlačené v porovnaní s príkladom 2.Waste water with chemical oxygen demand COD = 34,800 mg / l with a methanol content of 0.1% by weight. with a temperature of 110 ° C, was continuously fed into a mixing flask where water was added in an amount of 10% by weight. to said waste water. Further, toluene was added to the flask in an amount of 2% by weight. to said waste water. The residence time of the emulsions in the flask was 2 minutes. The toluene phase was separated in a separatory funnel and had a solids content of 9.6 wt. Dry matter analysis showed that it was 95% 4-aminodiphenylamine, the remainder being diphenylamine derivatives. Filtration of the waste water through a frit S 4 for 48 hours and after cooling to room temperature showed that the precipitated insoluble matter was less than 0.1 mg / l. COD cr waste water after extraction with toluene was 26 140 mg / l with respect to the raw sewage. The treated waste water was neutralized with 31% hydrochloric acid to pH = 6.5 and the separated chemical sludge was collected at 1.5 g / l. These waste waters have a chemical oxygen demand COD of Cr = 20,820 mg / l and have been injected into the laboratory model of the aerator of the wastewater treatment plant. At different levels of aeration, it was found that the treatment of the treated waste condensation was significantly suppressed compared to Example 2.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS867189A CS256581B1 (en) | 1986-10-06 | 1986-10-06 | Method of waste waters cleaning from n-phenyl-n-isopropyl-p-phenylendiamine production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS867189A CS256581B1 (en) | 1986-10-06 | 1986-10-06 | Method of waste waters cleaning from n-phenyl-n-isopropyl-p-phenylendiamine production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS718986A1 CS718986A1 (en) | 1987-08-13 |
| CS256581B1 true CS256581B1 (en) | 1988-04-15 |
Family
ID=5420567
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS867189A CS256581B1 (en) | 1986-10-06 | 1986-10-06 | Method of waste waters cleaning from n-phenyl-n-isopropyl-p-phenylendiamine production |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS256581B1 (en) |
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1986
- 1986-10-06 CS CS867189A patent/CS256581B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS718986A1 (en) | 1987-08-13 |
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