CS266960B1 - Method of waste hydrogen chloride treatment - Google Patents
Method of waste hydrogen chloride treatment Download PDFInfo
- Publication number
- CS266960B1 CS266960B1 CS865222A CS522286A CS266960B1 CS 266960 B1 CS266960 B1 CS 266960B1 CS 865222 A CS865222 A CS 865222A CS 522286 A CS522286 A CS 522286A CS 266960 B1 CS266960 B1 CS 266960B1
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- CS
- Czechoslovakia
- Prior art keywords
- acid
- methyl
- hydrochloric acid
- neutralization
- waste hydrochloric
- Prior art date
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000002699 waste material Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 title description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title description 2
- 229920000867 polyelectrolyte Polymers 0.000 claims abstract description 6
- 238000004062 sedimentation Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 15
- 239000005574 MCPA Substances 0.000 claims description 12
- WHKUVVPPKQRRBV-UHFFFAOYSA-N Trasan Chemical compound CC1=CC(Cl)=CC=C1OCC(O)=O WHKUVVPPKQRRBV-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- QJVXBRUGKLCUMY-UHFFFAOYSA-N 2-(2-methylphenoxy)acetic acid Chemical compound CC1=CC=CC=C1OCC(O)=O QJVXBRUGKLCUMY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims description 3
- SEGKFMXJNIEDQN-UHFFFAOYSA-N 2-(2,4-dichloro-6-methylphenoxy)acetic acid Chemical compound CC1=CC(Cl)=CC(Cl)=C1OCC(O)=O SEGKFMXJNIEDQN-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 239000011777 magnesium Substances 0.000 abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 6
- 235000019738 Limestone Nutrition 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000006028 limestone Substances 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- LCPDWSOZIOUXRV-UHFFFAOYSA-N phenoxyacetic acid Chemical class OC(=O)COC1=CC=CC=C1 LCPDWSOZIOUXRV-UHFFFAOYSA-N 0.000 description 3
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- WHLKFTSLSDHFMU-UHFFFAOYSA-N 2-(2-chloro-6-methylphenoxy)acetic acid Chemical compound CC1=CC=CC(Cl)=C1OCC(O)=O WHLKFTSLSDHFMU-UHFFFAOYSA-N 0.000 description 1
- OPHKGEDQTWIJEX-UHFFFAOYSA-N 2-methylphenol;hydrochloride Chemical class Cl.CC1=CC=CC=C1O OPHKGEDQTWIJEX-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
Odpadná kyselina chlorovodíková sa predneutralizuje s uhličitanom vápenatým a/alebo horečnatým a doneutralizuje sa s hydroxidom vápenatým v přítomnosti polyelektrolytu. Vyzrážané nečistoty sa oddelia sedimentáciou.Waste hydrochloric acid was added pre-neutralizes with calcium carbonate and / or magnesium and is neutralized with hydroxide calcium in the presence of polyelectrolyte. The precipitated impurities are separated by sedimentation.
Description
Vynález sa týká neutralizácie odpadnej kyseliny chlorovodíkovej, vznikájúcej pri výroběThe invention relates to the neutralization of waste hydrochloric acid produced during production
2-metyl-4-chlórfenoxyoctovej kyseliny:2-methyl-4-chlorophenoxyacetic acid:
2-metyl-4-chlórfenoxyoctová kyselina sa najčastejšie připravuje chloráciou 2-metylfenoxyoctovej kyseliny plynným chlórom alebo chlórňanom sodným. Chloráciu s chlórňanom sodným v přítomnosti minerálnej kyseliny a získanie 2-metyl-4-chlórfenoxyoctovej kyseliny popisuje AO 179 200. Pri výrobě odpadá minerálna kyselina, najčastejšie kyselina chlorovodíková, ktorá je znečistěná fenoxyoctovými kyselinami, ako sú kyseliny 2-metylfenoxyoctová, 2-metyl-4-chlórfenoxyoctová, 2-metyl-6-chlórfenoxyoctová, 2-metyl-4,6-dichlórfenoxyoctová, minerálnymi solami, predovšetkým chloridom sodným, chlórderivátmi 2-metylfenolu. Hodnota pH odpadnej kyseliny je 0 až 2, a to z toho důvodu, že vysrážaná 2-metyl-4-chlórfenoxyoctová kyselina je z nej lahko filtrovatelná.2-Methyl-4-chlorophenoxyacetic acid is most often prepared by chlorination of 2-methylphenoxyacetic acid with chlorine gas or sodium hypochlorite. Chlorination with sodium hypochlorite in the presence of mineral acid and recovery of 2-methyl-4-chlorophenoxyacetic acid is described in AO 179 200. Mineral acid, most often hydrochloric acid, which is contaminated with phenoxyacetic acids such as 2-methylphenoxyacetic acid, 2-methyl- 4-chlorophenoxyacetic acid, 2-methyl-6-chlorophenoxyacetic acid, 2-methyl-4,6-dichlorophenoxyacetic acid, mineral salts, in particular sodium chloride, 2-methylphenol chloride derivatives. The pH of the waste acid is 0 to 2, because the precipitated 2-methyl-4-chlorophenoxyacetic acid is easily filterable therefrom.
Pri využití a spracovaní odpadnej kyseliny sú problémy, vzhladom k tomu, že je takmer nasýtená anorganickými solami a má malú koncentráciu minerálnych kyselin. Ako odpad sa nemůže vypúšťať do kanalizácie, pretože vodohospodářské orgány súhlasia iba s vypúštaním po neutralizovaní na hodnotu pH 6 až 8. Najjednoduchšia neutralizácia je s lúhmi, predovšetkým s NaOH alebo Ca(OH)2< Určitá nevýhoda je tu prudká změna hodnory pH v blízkosti ekvivalentného bodu pri hodnote pH 7, čo může vyvolávat ťažkosti v priemyselnom meradle.There are problems in the use and processing of waste acid, due to the fact that it is almost saturated with inorganic salts and has a low concentration of mineral acids. It cannot be discharged as sewage, as water authorities only agree to discharge after neutralization to pH 6 to 8. The simplest neutralization is with lyes, especially NaOH or Ca (OH) 2 < A certain disadvantage here is a sharp change in the pH value in the vicinity equivalent point at pH 7, which can cause difficulties on an industrial scale.
Vyššie uvedené nedostatky sú zmiernené spůsobom úpravy odpadnej kyseliny chlorovodíkovej z výroby 2-metyl-4-chlórfenoxyoctovej kyseliny, podstata ktorého spočívá v tom, že sa odpadná kyselina chlorovodíková predneutralizuje s uhličitanom vápenatým a/alebo horečnatým na hodnotu pH 2 až 6,5 a doneutralizuje sa s hydroxidem vápenatým v přítomnosti polyelektrolytu. Polyelektrolyt sa přidává na lepšiu koaguláciu vyzrážaných častí a urýchlenie ich sedimentácie.The above drawbacks are alleviated by the method of treating waste hydrochloric acid from the production of 2-methyl-4-chlorophenoxyacetic acid, which consists in pre-neutralizing the waste hydrochloric acid with calcium and / or magnesium carbonate to a pH of 2 to 6.5 and done with calcium hydroxide in the presence of a polyelectrolyte. The polyelectrolyte is added to better coagulate the precipitated parts and accelerate their sedimentation.
Výhodou spůsobu podlá vynálezu je, že sa na predneutralizovanie kyseliny chlorovodíkovej použijú poměrně lačné suroviny, ktoré sa nachádzajú bežne v prírode ako vápenec, alebo dolomit. Výhodou uvedených látok je, že sú prakticky nerozpustné vo vodě a že prebytkom vápenca alebo dolomitu nie je možné prejsť do alkalickéj oblasti hodnoty pH. Doneutralizácia s hydroxidem vápenatým sa robí, ak je požiadavky, aby výsledná hodnota pH bola v blízkosti 7 alebo nad hodnotou 7. Hodnotu pH po doneutralizovaní určujú pri vypúšťaní do vodných tokov příslušné vodohospodářské orgány. Niekedy sa hodnota pH po doneutralizovaní určí z toho, do akej miery sa majú z odpadnej kyseliny chlorovodíkovej odstániť znečisťujúce látky, například kationy Fe, Mg, Zn a pod. Výhodné je možné predneutralizáciu odpadnej kyseliny chlorovodíkovej robit vo výrobní 2-metyl-4-chlórfenoxyoctovej kyseliny a doneutralizáciu robit na centrálnej neutralizačnej stanici v podniku, po zmiešaní predneutralizovanej odpadnej kyseliny chlorovodíkovej s inými odpadnými vodami z iných výrobní podniku. Predneutralizovaná kyselina chlorovodíková je menej korozívna a z toho důvodu sú menšie nároky na materiál, z ktorého je zhotovené potrubie.An advantage of the process according to the invention is that relatively fasting raw materials, which are commonly found in nature, such as limestone or dolomite, are used for the pre-neutralization of hydrochloric acid. The advantage of these substances is that they are practically insoluble in water and that it is not possible to pass into the alkaline pH range with an excess of limestone or dolomite. Donated neutralization with calcium hydroxide is done if the resulting pH value is required to be close to 7 or above 7. The pH value after done-neutralization is determined by the relevant water authorities when discharged into watercourses. Sometimes the pH value after donation is determined by the extent to which contaminants, for example Fe, Mg, Zn cations and the like, are to be removed from the waste hydrochloric acid. Advantageously, the pre-neutralization of the waste hydrochloric acid can be done in the 2-methyl-4-chlorophenoxyacetic acid production and the neutralization can be done at the central neutralization station in the plant, after mixing the pre-neutralized waste hydrochloric acid with other effluents from other plants. Pre-neutralized hydrochloric acid is less corrosive and therefore the material from which the pipe is made is less demanding.
Příklad 1Example 1
Odpadná kyselina chlorovodíková z výroby 2-metyl-4-chlórfenoxyoctovej kyseliny podlá čs. AO 179 200 málo následovně zloženie:Waste hydrochloric acid from the production of 2-methyl-4-chlorophenoxyacetic acid according to MS. AO 179 200 has the following composition:
chlorovodík 1,8 % hmot.hydrogen chloride 1.8% by weight
fenoxyoctové kyseliny 4,1 g/1phenoxyacetic acid 4.1 g / l
Cl chlórderiváty 2-metylfenoluCl chlorine derivatives of 2-methylphenol
92,8 g/192.8 g / l
0,16 g/10.16 g / l
000 ml odpadnej kyseliny chlorovodíkovej sa zneutralizovalo s vápencem na hodnotu pH 3,1. Po oddělení vápenca sa k reakčnej zmesi přidalo 0,2 ml 0,1 % hmot, vodného gelu polyelektrolytu (Magnaflor). Potom sa s 5,5 % hmot, suspenziu Ca(OH)2 reakčná zmes zneutralizovala na hodnotu pH 7,2. Vysrážané nečistoty sa oddělili sedimentáciou.000 ml of waste hydrochloric acid were neutralized with limestone to pH 3.1. After separating the limestone, 0.2 ml of a 0.1% by weight aqueous polyelectrolyte gel (Magnaflor) was added to the reaction mixture. Then, with a 5.5% by weight suspension of Ca (OH) 2, the reaction mixture was neutralized to pH 7.2. The precipitated impurities were separated by sedimentation.
CS 266 960 BlCS 266 960 Bl
Příklad 2Example 2
Postupovalo sa podlá příkladu 1 s tým rozdielom, že sa odpadná kyselina chlorovodíková predneutralizovala na hodnotu pH 4,3. Potom sa reakčný roztok zmiešal s odpadnými vodami z výrobní CHZJD, aby výsledný roztok představoval chemicky znečistenú vodu, ktorá v súčasnosti v CHZJD vzniká a ktorá mala následovně zloženie:The procedure of Example 1 was followed, except that the waste hydrochloric acid was pre-neutralized to pH 4.3. Then, the reaction solution was mixed with the wastewater from the production CHZJD, so that the resulting solution was chemically contaminated water, which is currently formed in the CHZJD and which had the following composition:
,2 ml 0,1 % hmot, vodného gelu polyelektrolytu (Magnoflor) a potom sa přidala 5,5 % hmot, suspenzia Ca(OH)?. Hodnota pH po neutralizá2+ 3+ 3+ 2+ cii bola 7,6. Vysrážené nečistoty, predovšetkým hydralované oxidy Zn , Fe , AI , Mg sa oddělili sedimentáciou., 2 ml of 0.1% by weight of an aqueous polyelectrolyte gel (Magnoflor) and then 5.5% by weight of a suspension of Ca (OH) ? . The pH after neutralization 2 + 3+ 3+ 2+ cii was 7.6. The precipitated impurities, especially the hydrated oxides of Zn, Fe, Al, Mg, were separated by sedimentation.
Příklad 3Example 3
Postupovalo sa podlá příkladu 1 s tým rozdielom, že sa odpadná kyselina chlorovodíková predneutralizovala s mikromletým magnezitom na hodnotu pH 6,4. Hodnota pH po doneutralizovaní bola 7,4. Vyzrážené nečistoty sa odstránili sedimentáciou.The procedure of Example 1 was followed, except that the waste hydrochloric acid was pre-neutralized with micronized magnesite to pH 6.4. The pH after doneutralization was 7.4. Precipitated impurities were removed by sedimentation.
Vynález nájde uplatnenie pri neutralizávii odpadnej kyseliny chlorovodíkovéj vznikajúcej pri výrobě kyseliny 2-metyl-4-chlórfenoxyoctovej. Výhodné je možno predneutralizovať odpadnú kyselinu chlorovodíková vo výrobní 2-metyl-4-chlórfenoxyoctovej kyseliny a doneutralizáciu urobit na centrálnej neutralizačnej stanici kyslých odpadných vód.The invention finds application in the neutralization of waste hydrochloric acid formed in the production of 2-methyl-4-chlorophenoxyacetic acid. Preferably, the waste hydrochloric acid can be pre-neutralized in the production of 2-methyl-4-chlorophenoxyacetic acid and the neutralization can be done at a central acid waste water neutralization station.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS865222A CS266960B1 (en) | 1986-07-09 | 1986-07-09 | Method of waste hydrogen chloride treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS865222A CS266960B1 (en) | 1986-07-09 | 1986-07-09 | Method of waste hydrogen chloride treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS522286A1 CS522286A1 (en) | 1989-06-13 |
| CS266960B1 true CS266960B1 (en) | 1990-01-12 |
Family
ID=5396695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS865222A CS266960B1 (en) | 1986-07-09 | 1986-07-09 | Method of waste hydrogen chloride treatment |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS266960B1 (en) |
-
1986
- 1986-07-09 CS CS865222A patent/CS266960B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS522286A1 (en) | 1989-06-13 |
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