CS235355B1 - Method of 2-methyl-4-chlorphenoxyacetic acid preparation - Google Patents
Method of 2-methyl-4-chlorphenoxyacetic acid preparation Download PDFInfo
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- CS235355B1 CS235355B1 CS618782A CS618782A CS235355B1 CS 235355 B1 CS235355 B1 CS 235355B1 CS 618782 A CS618782 A CS 618782A CS 618782 A CS618782 A CS 618782A CS 235355 B1 CS235355 B1 CS 235355B1
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- sulfuric acid
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- WHKUVVPPKQRRBV-UHFFFAOYSA-N Trasan Chemical compound CC1=CC(Cl)=CC=C1OCC(O)=O WHKUVVPPKQRRBV-UHFFFAOYSA-N 0.000 title claims description 18
- 238000000034 method Methods 0.000 title description 10
- 238000002360 preparation method Methods 0.000 title description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 46
- 239000005574 MCPA Substances 0.000 claims description 17
- 238000005660 chlorination reaction Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- QJVXBRUGKLCUMY-UHFFFAOYSA-N 2-(2-methylphenoxy)acetic acid Chemical compound CC1=CC=CC=C1OCC(O)=O QJVXBRUGKLCUMY-UHFFFAOYSA-N 0.000 claims description 8
- 235000002639 sodium chloride Nutrition 0.000 claims description 8
- 159000000000 sodium salts Chemical class 0.000 claims description 7
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 239000011686 zinc sulphate Substances 0.000 claims description 3
- 235000009529 zinc sulphate Nutrition 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- -1 nitro- Chemical class 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000005708 Sodium hypochlorite Substances 0.000 description 5
- LCPDWSOZIOUXRV-UHFFFAOYSA-N phenoxyacetic acid Chemical class OC(=O)COC1=CC=CC=C1 LCPDWSOZIOUXRV-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 5
- 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 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- PIIZYNQECPTVEO-UHFFFAOYSA-N 4-nitro-m-cresol Chemical compound CC1=CC(O)=CC=C1[N+]([O-])=O PIIZYNQECPTVEO-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RKMNQXFECVRTNI-UHFFFAOYSA-N 1-methylcyclohexa-2,4-dien-1-ol Chemical compound CC1(O)CC=CC=C1 RKMNQXFECVRTNI-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- VQLFVRAWSGUGAX-UHFFFAOYSA-N 2-(4-ethyl-2-methylphenoxy)acetic acid Chemical compound C(C(=O)O)OC1=C(C=C(CC)C=C1)C VQLFVRAWSGUGAX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- SGBQSEGKEOXZFT-UHFFFAOYSA-N CC1=C(OCC(=O)O)C=CC=C1.[K].[Na] Chemical compound CC1=C(OCC(=O)O)C=CC=C1.[K].[Na] SGBQSEGKEOXZFT-UHFFFAOYSA-N 0.000 description 1
- SWSLZOGIGIOJGN-UHFFFAOYSA-N COOC(C(=O)O)C Chemical compound COOC(C(=O)O)C SWSLZOGIGIOJGN-UHFFFAOYSA-N 0.000 description 1
- DKHJWWRYTONYHB-UHFFFAOYSA-N CPP Chemical compound OC(=O)C(C)OC1=CC=C(Cl)C=C1 DKHJWWRYTONYHB-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- HKNMVNAPCMXVTR-UHFFFAOYSA-M sodium;2-(2-methylphenoxy)acetate Chemical compound [Na+].CC1=CC=CC=C1OCC([O-])=O HKNMVNAPCMXVTR-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Vynález sa týká přípravy 2-metyl-4-chlórfeinoxyoctovej kyseliny chloráciou 2-metylfenoxyoctovej kyseliny a jej sodnej soli chlornanom sodným,.The present invention relates to the preparation of 2-methyl-4-chlorophenoxyacetic acid by chlorination of 2-methylphenoxyacetic acid and its sodium salt with sodium hypochlorite.
Kyselina 2-metyl-4-ehlárfenoxyoctová a jej soli sa používajú ako velmi účinné herbicidy. Najčastejšie sa připravuje chloráciou 2-metylřemoxyoctovej kyseliny plynným chlórom pri teplote 95 až 105 °C, ako je opísané v ČSSR patente 91160. Kontinuálny sposob chlorácie sodnej, draseilnej alebo sodnodraselnoj soli 2-metylfenoxyoctovej kyseliny vo vodinom roztoku je opísaný v ČSSR patente 99 892, kontinuálny sposob chlorácie voTnej 2-metylfenoxyoctovej kyseliny plynným chlórom opisuje ČSSR patent 107 807. Možnost kombinácie chlorácie 2-metylfenoxyootovej kyseliny plynným chlórom s následným dochlórovaním chlórnanom uvádza CSSR AO 172 188. Chloráciu 2-metylfenoxyoctovej kyseliny plynným chlórom pri hodnotě pH 4 až 6 opisuje francúzsky pait. 1 116 266. Chloráciu vodným roztokom chlórnanu sodného připraveného vopred aleboi „in šitu“ v reakčnej zmesi pri teplote 50 °C opisuje pat. V. Británie 722 625. Chloráciu suspendovanej 2-metylfemoxyoctovej kyseliny pri hodnotě pH rovnej 1 v heterogénnej fáze za přítomnosti kyseliny chlórovodíkovej chlornanem sodným pri teplote 20 °C opisuje DAS 1 027 680. Spósob založený na působení hydroxidu sodného alebo uhličitanu sodného na vodný roztok sodnej soli 2-metylfenoxyoctovej kyseliny a chloráciu chlórom opisuje pat. USA číslo 2 770 651. Chlorácia sodnej soli 2-metylfenoxyoctovej kyseliny chlórom v přítomnosti hydroulhličitanu je opisaná v pat, V. Británie 855 504. Výrobu 2-metyl-4-chlórfemoxyoctovej kyseliny pomocou chlórnanu sodného1 v přítomnosti minerálnej alebo karboxylovej kyseliny, výrobu 2-metyl-4-chlórfenoxyoctovej kyseliny chloráciou sodnej soli 2-metylfenoxyoctovej kyseliny vyzrážaním s přebytkem vodného roztoku minerálnej kyseliny opisuje CSSR AO 179 200.2-Methyl-4-ethylphenoxyacetic acid and its salts are used as highly effective herbicides. Most often it is prepared by chlorination of 2-methyl-methoxyoxyacetic acid with chlorine gas at a temperature of 95-105 ° C, as described in USSR Patent 91160. A continuous process for chlorination of sodium, potassium or sodium potassium 2-methylphenoxyacetic acid in a water solution is described in USSR Patent 99,892; The continuous chlorination method of chlorine-free 2-methylphenoxyacetic acid is described in Czechoslovakia's patent 107,807. Pait. Chlorination with an aqueous solution of sodium hypochlorite prepared previously or "in situ" in the reaction mixture at 50 ° C is described in U.S. Pat. UK 722 625. DAS 1 027 680 describes the chlorination of suspended 2-methylphemoxyacetic acid at a pH of 1 in heterogeneous phase in the presence of hydrochloric acid at 20 ° C. The method is based on the action of sodium hydroxide or sodium carbonate on an aqueous sodium solution. salts of 2-methylphenoxyacetic acid and chlorination chlorine are described in U.S. Pat. No. 2,770,651. Chlorination of 2-methylphenoxyacetic acid sodium salt in the presence of bicarbonate is disclosed in U.S. Pat. No. 855,504. Production of 2-methyl-4-chlorophemoxyacetic acid using sodium hypochlorite 1 in the presence of mineral or carboxylic acid, production 2 -methyl-4-chlorophenoxyacetic acid by chlorination of the sodium salt of 2-methylphenoxyacetic acid by precipitation with an excess of an aqueous mineral acid solution is described in CSSR AO 179 200.
Uvedené nedostatky zmierňujú postup přípravy 2-roetyl-4-chlórfenoxyoctovej kyseliny chloráciou zmesi 2-metylfenoxyoctovej kyseliny a jej sodnej soli v prostředí vodného roztoku kyseliny sírovej s následným přidáním kyseliny sírovej k rozteku alebo· suspenzii reakčného produktu a oddělením 2-metyl-4-chlórfenoxyoctovej kyseliny od matečného roztoku, podstatou ktorého je to, že kyselina sírová o koncentrácii 3 až 50 % hmotnostných obsahuje hydrogénsírain sodný, síran zinočinatý, síran sodný, dusičnan sodný, chlorid sodný a kyselinu dusičná súhrnne v množstve 3 až 40 % hmotnostných, tiež deriváty fenolu, najčastejšie 3-metyl-4-nitrofenol, 3-metylfenol a ich nitro-, nitrozo- a sulfoderiváty súhrnne v množstve 5 až 2500 mg, pričom množstvo1 kyseliny sírovej je 0,8 až 1,8 molekvivaleratov na súčeit molekvivalentov sodnej soli 2-metyl-4-chlórfenoxyoctovej kyseliny v chlórnanu sodného vzniknutého hydroxidu sodného.The above drawbacks alleviate the process for preparing 2-methyl-4-chlorophenoxyacetic acid by chlorination of a mixture of 2-methylphenoxyacetic acid and its sodium salt in an aqueous sulfuric acid solution followed by addition of sulfuric acid to the solution or suspension of the reaction product and separation of 2-methyl-4-chlorophenoxyacetic acid acid from the mother liquor, which is characterized in that the sulfuric acid at a concentration of 3 to 50% by weight contains sodium hydrogen sulphate, zinc sulphate, sodium sulphate, sodium nitrate, sodium chloride and nitric acid in aggregate of 3 to 40% by weight, also phenol derivatives , most commonly 3-methyl-4-nitrophenol, 3-methylphenol and their nitro-, nitroso- and sulfoderivatives in total in the amount of 5 to 2500 mg, the amount 1 of sulfuric acid being 0.8 to 1.8 mol equivalents per sum of mol equivalents of sodium salt 2 of methyl-4-chlorophenoxyacetic acid in sodium hypochlorite formed sodium hydroxide.
Matečný roztok získaný po oddělení 2-metyl-4-chlórfenoxyoctovej kyseliny je možné použiť opatovne po doplnění na povodně množstvo kyseliny sírovej v ďalšej várke opakovaného postupu.The mother liquor obtained after the separation of 2-methyl-4-chlorophenoxyacetic acid can be used carefully after the flood has been replenished with an amount of sulfuric acid in the next batch of the repeated process.
Prínosoim opísainého postupu přípravy a izolácie 2-metyl-4-chlórfenoxyoctovej kyseliny je skutočnosť, že vzniká podstatné menej odpadných vod s vyšším obsahom anorganických a organických solí, tiež s nižším obsahom 2-metyl-4-chlórfenoxyoetovej kyseliny. Anorganické a organické soli znižujú podstatné rozpustnost produktu 2-metyl-4-chlóroctovej kyseliny v matečnom roztoku, čím sa dosiahne vyšší výťažok.One advantage of the process described above for the preparation and isolation of 2-methyl-4-chlorophenoxyacetic acid is that substantially less waste water is produced with a higher content of inorganic and organic salts, also with a lower content of 2-methyl-4-chlorophenoxyacetic acid. Inorganic and organic salts reduce the substantial solubility of the 2-methyl-4-chloroacetic acid product in the mother liquor, resulting in a higher yield.
Matečný roztok odpadajúci pri tomto· postupe má menšiu chemickú spotřebu kyslíka ako matečný roztok pri póvodnom postupe. Ekonomickým prínosom je menšia spotřeba kyseliny sírovej, maviac móže byť použitá kyselina sírová, ktorá je znečistěná anorganickými alebo organickými sofami.The mother liquor leaving this process has less chemical oxygen consumption than the mother liquor in the original process. The economic benefit is less sulfuric acid consumption, and sulfuric acid contaminated with inorganic or organic salts may be used.
Příklad 1Example 1
K 940 g vodného roztoku obsahujúoeho 0,4 % hmotnostného 2-metylfenoxyoctovej kyseliny a 13 % hmotnostných sodnej soliTo 940 g of an aqueous solution containing 0,4% by weight of 2-methylphenoxyacetic acid and 13% by weight of sodium salt
2- metylfenoxyoctovej kyseliny sa za miešania přidalo 620 g vodného roztoku 12,7 % hmotnostného chlórnanu sodného a 180 g kyseliny sírovej o koncentrácii 35 % hmotnostných takou rýchlosťou, aby teplota nepřekročila 45 °C. Po přidaní celého, množstva kyseliny sírovej sa zrnes 1 hodinu miešala. Vzniknutý roztok sa vlial do 700 g kyseliny sírovej o koncentrácii 9,1 % hmotinostného. Vyzrážaná 2-metyl-4-chlórfenoxyoctová kyselina sa odfiltrovala a premyla 500 mil vody. Získalo sa 131,1 g produktu s obsahom 91,6 °/o_ hmotnostného 2-metyl-4-chlórfenoxyoctovej kyseliny. Filtrátu bolo 2164 g s konce,nitráciou 9,1 g/1 fenoxyoctových kyselin (jedná sa o zrnes 2-metyl-4-chlórfenoxyoctovej kyseliny, 2-metyl-4,6-dichlórfenoxyoctovej kyseliny.2-Methylphenoxyacetic acid was added with stirring 620 g of an aqueous solution of 12.7 wt% sodium hypochlorite and 180 g of sulfuric acid at a concentration of 35 wt% at such a rate that the temperature did not exceed 45 ° C. After all of the sulfuric acid was added, the mixture was stirred for 1 hour. The resulting solution was poured into 700 g of 9.1 wt% sulfuric acid. The precipitated 2-methyl-4-chlorophenoxyacetic acid was filtered off and washed with 500 ml of water. 131.1 g of a product containing 91.6% by weight of 2-methyl-4-chlorophenoxyacetic acid were obtained. The filtrate was 2164 g with end, nitration of 9.1 g / l phenoxyacetic acids (a mixture of 2-methyl-4-chlorophenoxyacetic acid, 2-methyl-4,6-dichlorophenoxyacetic acid).
Příklad 2Example 2
Postupovalo sa podlá příkladu 1 s tým rozdieloím, že v chlorácii sa použila kyselina sírová v množstve 720 g o koncentrácii 8,8 percenta hmotnostného s obsahom 3,6 % hmotnostného hydrosírainu sodného, 0,4 % hmotnostného kyseliny dusičnej, 520 mg/1The procedure was as described in Example 1 except that in chlorination, sulfuric acid of 720 g at a concentration of 8.8% by weight containing 3.6% by weight sodium hydrosulphate, 0.4% by weight nitric acid, 520 mg / l was used.
3- metyl-4-nitrofenolu a 310 mg/1 3-m©tylfenolu. Na zrážanie sa použilo 285 g kyseliny sírovej o koncentrácii 22,1 % hmotnostného s obsahom 8,4 % hmotnostného hydrosírainu sodného, 1,2 °/o hmotnostného kyseliny dusičnej, 1470 mg/1 3-metyl-4-nitrofenolu a 1320 mg/1 metylfenolu. Získalo· sa 132,4 g produktu s obsahom 92,5 % hmotnostného 2-metyl-4-chlórfenoxyoctovej ky233353 seliiny. Filtrátu bolo 2284 g s konceotráciou 5,6 g/1 fenoxyoctových kyselím, ako v příklade 1.3-methyl-4-nitrophenol and 310 mg / L of 3-methylphenol. 285 g of sulfuric acid at a concentration of 22.1% by weight containing 8.4% by weight of sodium hydrosulphate, 1.2% by weight of nitric acid, 1470 mg / l of 3-methyl-4-nitrophenol and 1320 mg were used for the precipitation. 1 methylphenol. 132.4 g of a product containing 92.5% by weight of 2-methyl-4-chlorophenoxyacetic acid 232333 seline were obtained. The filtrate was 2284 g with a 5.6 g / l phenoxyacetic acid endpoint as in Example 1.
Příklad 3Example 3
Postupovalo sa podl'a příkladu 2 s tým rozdielom, že pri chlorácii použitá kyselina sírová sa připravila riedením· kyseliny sírovej s filtrá tom z příkladu 2. Výsledné zložemie kyseliny sírovej boto: 9,6 °/o hmotnostného kyseliny sírovej, 5,2 % hmot. hydrosíranu sodného, 0,5 % hmotnostného kyseliny dusičnej a 520 mg/1 3-metyl-4-mltrofenolu a bola použitá v množstve 660 g. Získalo· sa 134,5 g produlktu s obsahom 92,7 % hmotnostného 2-metyl-4-chlórfenoxyoetovej kyseliny. Filtrátu bolo 2215 g a obsahoval 3,49 g/1 fenoxyoctových kyselin ako v příklade 1.The procedure of Example 2 was followed except that the sulfuric acid used in the chlorination was prepared by diluting the sulfuric acid with the filter of Example 2. The resulting sulfuric acid composition was 9.6% by weight sulfuric acid, 5.2% by weight. wt. sodium hydrosulfate, 0.5 wt% nitric acid and 520 mg / L of 3-methyl-4-mltrophenol were used in an amount of 660 g. 134.5 g of a product having a content of 92.7% by weight of 2-methyl-4-chlorophenoxy-acetic acid were obtained. The filtrate was 2215 g and contained 3.49 g / l phenoxyacetic acids as in Example 1.
Příklad 4Example 4
Postupovalo sa podía příkladu 1 s tým rozdielom, že na zrážanie sa použila kyselina sírová o zložení 11,2 % hmotnostného kyseliny sírovej, 12,2 % hmotnostného hydrosíranu sodného, 1,2 % hmotnostného síranu zinočnatého· v množstve 900 g. Získalo; sa 132,1 g produktu s obsahom 92,4 % hmotnostného 2-metyl-4-chlórfenoxyocto.vej kyseliny. Filtrátu bolo 2342 g a obsahoval 4,9 g/1 fenoxyoctovýoh kyselin ako v příklade 1.The procedure of Example 1 was followed except that sulfuric acid of 11.2% by weight sulfuric acid, 12.2% by weight sodium hydrosulfate, 1.2% by weight zinc sulphate in an amount of 900 g was used. yield; 132.1 g of product containing 2-methyl-4-chlorophenoxyacetic acid containing 92.4% by weight. The filtrate was 2342 g and contained 4.9 g / l phenoxyacetic acids as in Example 1.
Vynález je možné použit pri přípravě 2-metyl-4-chlóríenoxyoctovej kyseliny. Je možné použiť kyselinu sirovu is obsahom anorganických solí a organických nečistot; odpadajúcich pri iných výrobných procesoch; ktorých únosnost je přípustná.The invention is applicable to the preparation of 2-methyl-4-chlorophenoxyacetic acid. Sulfuric acid containing inorganic salts and organic impurities may be used; falling off in other manufacturing processes; whose bearing capacity is permissible.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS618782A CS235355B1 (en) | 1982-07-25 | 1982-07-25 | Method of 2-methyl-4-chlorphenoxyacetic acid preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS618782A CS235355B1 (en) | 1982-07-25 | 1982-07-25 | Method of 2-methyl-4-chlorphenoxyacetic acid preparation |
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| Publication Number | Publication Date |
|---|---|
| CS235355B1 true CS235355B1 (en) | 1985-05-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CS618782A CS235355B1 (en) | 1982-07-25 | 1982-07-25 | Method of 2-methyl-4-chlorphenoxyacetic acid preparation |
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| CS (1) | CS235355B1 (en) |
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1982
- 1982-07-25 CS CS618782A patent/CS235355B1/en unknown
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