CS265751B1 - Method of 2-methyl-4-chlorphenoxy acetic acid's dimethylamine salt production - Google Patents
Method of 2-methyl-4-chlorphenoxy acetic acid's dimethylamine salt production Download PDFInfo
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- CS265751B1 CS265751B1 CS845976A CS597684A CS265751B1 CS 265751 B1 CS265751 B1 CS 265751B1 CS 845976 A CS845976 A CS 845976A CS 597684 A CS597684 A CS 597684A CS 265751 B1 CS265751 B1 CS 265751B1
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- methyl
- acid
- chlorophenoxyacetic acid
- dimethylamine
- chlorophenoxyacetic
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- WHKUVVPPKQRRBV-UHFFFAOYSA-N Trasan Chemical compound CC1=CC(Cl)=CC=C1OCC(O)=O WHKUVVPPKQRRBV-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 125000002147 dimethylamino group Chemical class [H]C([H])([H])N(*)C([H])([H])[H] 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title claims description 7
- 239000005574 MCPA Substances 0.000 claims abstract description 35
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 20
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 19
- 239000011707 mineral Substances 0.000 claims abstract description 19
- PKAUICCNAWQPAU-UHFFFAOYSA-N 2-(4-chloro-2-methylphenoxy)acetic acid;n-methylmethanamine Chemical compound CNC.CC1=CC(Cl)=CC=C1OCC(O)=O PKAUICCNAWQPAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 4
- 230000002363 herbicidal effect Effects 0.000 claims abstract description 4
- 239000004009 herbicide Substances 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 230000003472 neutralizing effect Effects 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 2
- HKNMVNAPCMXVTR-UHFFFAOYSA-M sodium;2-(2-methylphenoxy)acetate Chemical compound [Na+].CC1=CC=CC=C1OCC([O-])=O HKNMVNAPCMXVTR-UHFFFAOYSA-M 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims 2
- 239000000292 calcium oxide Substances 0.000 claims 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 14
- 150000007513 acids Chemical class 0.000 abstract description 7
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- HABAPWZXRLIZDL-UHFFFAOYSA-N 2-chloro-2-phenoxyacetic acid Chemical compound OC(=O)C(Cl)OC1=CC=CC=C1 HABAPWZXRLIZDL-UHFFFAOYSA-N 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 abstract 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract 1
- 150000001342 alkaline earth metals Chemical class 0.000 abstract 1
- PMPOPSWETLDYSC-UHFFFAOYSA-N azanium;2-(4-chloro-2-methylphenoxy)acetate Chemical compound [NH4+].CC1=CC(Cl)=CC=C1OCC([O-])=O PMPOPSWETLDYSC-UHFFFAOYSA-N 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 238000005660 chlorination reaction Methods 0.000 description 11
- QJVXBRUGKLCUMY-UHFFFAOYSA-N 2-(2-methylphenoxy)acetic acid Chemical compound CC1=CC=CC=C1OCC(O)=O QJVXBRUGKLCUMY-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- FLNGZLIXHKKSGN-UHFFFAOYSA-N 2-(4-chloro-1-methylcyclohexa-2,4-dien-1-yl)oxyacetic acid Chemical compound OC(=O)COC1(C)CC=C(Cl)C=C1 FLNGZLIXHKKSGN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-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
- RHLLDTPGTFRJDJ-UHFFFAOYSA-N OCl.OCl Chemical compound OCl.OCl RHLLDTPGTFRJDJ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 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
- 238000011437 continuous method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 oxides Chemical class 0.000 description 1
- LCPDWSOZIOUXRV-UHFFFAOYSA-N phenoxyacetic acid Chemical class OC(=O)COC1=CC=CC=C1 LCPDWSOZIOUXRV-UHFFFAOYSA-N 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Rieši sa výroba dimetlylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny, pričom na neutralizáciu minerálnych kyselin, ktoré obsahuje 2-metyl-4-chlc5rfenoxyoctová kyselina sa použije amoniak, uhličitan amonný, hydroxid alebo kysličník alkalického kovu alebo kovu alkalických zemin. 2-metyl-4- -chlórfenoxyoctová kyselina sa potom neutralizuje vodným roztokom dimetylaminu. Riešenie je možné použiť pri výrobě dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny, ktorá sa používá ako herbicid.The production of the dimethyl amine salt is solved 2-methyl-4-chlorophenoxyacetic acid; to neutralize mineral acids that contains 2-methyl-4-chloro-phenoxyacetic acid ammonia, ammonium carbonate, alkali metal hydroxide or oxide or alkaline earth metal. 2-methyl-4- The chlorophenoxyacetic acid is then neutralized dimethylamine aqueous solution. The solution can be used in the production of dimethylamine 2-methyl-4-chlorophenoxyacetic acid salt acid which is used as a herbicide.
Description
2-metyl-4-chlórfenoxyoctovej kyseliny, pričom na neutralizáciu minerálnych kyselin, ktoré obsahuje 2-metyl-4-chlc5rfenoxyoctová kyselina sa použije amoniak, uhličitan amonný, hydroxid alebo kysličník alkalického kovu alebo kovu alkalických zemin. 2-metyl-4-chlórfenoxyoctová kyselina sa potom neutralizuje vodným roztokom dimetylaminu. Riešenie je možné použiť pri výrobě dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny, ktorá sa používá ako herbicid.2-methyl-4-chlorophenoxyacetic acid, wherein ammonia, ammonium carbonate, an alkali metal or alkaline earth metal hydroxide or oxide are used to neutralize the mineral acids containing 2-methyl-4-chlorophenoxyacetic acid. The 2-methyl-4-chlorophenoxyacetic acid is then neutralized with an aqueous dimethylamine solution. The solution can be used in the preparation of the dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid, which is used as a herbicide.
CS 265 751 B1CS 265 751 B1
Vynález sa týká výroby dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny.The invention relates to the preparation of the dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid.
Kyselina 2-metyl-4-chlórfenoxyoctová a jej soli sa používajú ako velmi účinné herbicidy. Najčastejšie sa připravuje chloráciou 2-metylfenoxyoctovej kyseliny plynným chlórom pri teplote 95 až 105 °C, ako je opisané v ČSSR patente 91 160. Kontinuálny spósob chlorácie sodnéj, draselnej alebo sodnodraselnej soli 2-metylfenoxyoctovej kyseliny vo vodnom roztoku je opísaný V ČSSR patente 99 892, kontinuálny spósob chlorácie volnéj 2-metylfenoxyoctovej kyseliny plynným chlórom opisuje ČSSR patent 107 807. Možnost kombinácie chlorácie 2-metylfenoxyoctovej kyseliny plynným chlórom s následným dochlórovanim chlórňanom uvádza ČSSR AO 172 188. Chloráciu 2-metylfenoxyoctovej kyseliny plynným chlórom pri hodnotě pH 4 až 6 opisuje francúzsky patent 1 116 266. Chloráciu vodným roztokom chlórňanu sodného připraveného vopred alebo in šitu v reakčnej zmesi pri teplote 50 °C opisuje patent'V. Británie 722 625. Chloráciu suspendovanéj 2-metylfenoxyoctovej kyseliny pri hodnotě pH rovnej 1 v hete rogénnej fáze za přítomnosti kyseliny chlorovodíkovéj chlórňanom sodným pri teplote 20 °C opisuje DAS 1 027 680. Chlorácia sodnej soli 2-metylfenoxyoctovej kyseliny chlórom v přítomnosti hydrouhličitanu je opísaná v patente V. Británie 855 504. Výrobu 2-metyl-4-chlórfenoxyoctovej kyseliny pomocou chlórňanu sodného v přítomnosti minerálnej alebo karboxylovej kyseliny, výrobu 2-metyl-4-chlórfenoxyoctovej kyseliny chloráciou sodnej soli 2-metylfenoxyoctovej kyseliny a ziskanie 2-metyl-4-chlórfenoxyoctovej kyseliny vyzrážanim s prebytkom vodného roztoku minerálnej kyseliny opisuje ČSSR AO 179 200.2-Methyl-4-chlorophenoxyacetic acid and its salts are used as highly effective herbicides. Most commonly it is prepared by chlorination of 2-methylphenoxyacetic acid with chlorine gas at a temperature of 95-105 ° C as described in USSR patent 91 160. A continuous process for chlorination of sodium, potassium or sodium potassium salt of 2-methylphenoxyacetic acid in aqueous solution is described in USSR patent 99,892 , a continuous method of chlorination of free 2-methylphenoxyacetic acid by chlorine gas is described in Czechoslovakia Patent 107,807. The possibility of combining chlorination of 2-methylphenoxyacetic acid with chlorine gas followed by hypochlorite hypochlorite is reported by ČSSR AO 172 188. Chlorination of 2-methylphenoxyacetic acid French patent 1 116 266. Chlorination with an aqueous solution of sodium hypochlorite prepared in advance or in situ in the reaction mixture at 50 ° C is described in U.S. Pat. Britain 722 625. The chlorination of suspended 2-methylphenoxyacetic acid at a pH of 1 in the hogenous phase in the presence of hydrochloric acid with sodium hypochlorite at 20 ° C is described in DAS 1 027 680. Chlorination of sodium salt of 2-methylphenoxyacetic acid by chlorine in the presence of bicarbonate U.S. Patent 855,504. Production of 2-methyl-4-chlorophenoxyacetic acid using sodium hypochlorite in the presence of mineral or carboxylic acid, production of 2-methyl-4-chlorophenoxyacetic acid by chlorination of the sodium salt of 2-methylphenoxyacetic acid and recovery of 2-methyl-4- of chlorophenoxyacetic acid by precipitation with an excess of an aqueous mineral acid solution is described in Czechoslovakia AO 179 200.
Nevýhodou přípravy podlá čs. AO 179 200 je, že sa 2-metyl-4-chlórfenoxyoctová kyselina získá z roztoku po chlorácii vyzrážením z přebytku minerálnej kyseliny, s následným odfiltrováním 2-metyl-4-chlórfenoxyoctovej kyseliny od matečného lúhu minerálnych kyselin.The disadvantage of preparation according to MS. AO 179 200 is that 2-methyl-4-chlorophenoxyacetic acid is recovered from the solution after chlorination by precipitation from an excess of mineral acid, followed by filtering 2-methyl-4-chlorophenoxyacetic acid from the mother liquor.
Filtračný koláč obsahuje 30 až 80 % hmot. fenoxyootových kyselin, pričom zvyšok do 100 % hmot. tvoří prevažne matečný roztok minerálnych kyselin s koncentráciou 0,2 až 2 í hmot. minerálnej kyseliny. Koncentrácia minerálnych kyselin v matečnom roztoku sa v uvedenom rozmedzí udržiava z toho dóvodu, že suspenzia 2-metyl-4-chlórfenoxyoctovej kyseliny je v tomto rozmedzí dobré filtrovatelná. Premývanie filtračného koláča sa nerobí z toho dóvodu, že 2-metyl-4-chlórfenoxyoctová kyselina je rozpustná vo vodě 2 až 10 g/1 (podlá teploty), čo móže zapříčinit straty produktu. Pri neutralizácii filtračného koláča neutralizačně činidlo okrem neutralizácie 2-metyl-4-chlórfenoxyoctovej kyseliny neutralizuje přednostně minerálně kyseliny, čím sa zapříčiňuje jeho strata. Toto je nevýhodné hlavně pri použití drahších neutralizaěných činidiel napr. dimetylaminu.The filter cake contains 30 to 80 wt. % of phenoxyootic acids, the remainder being up to 100 wt. it is predominantly a mother liquor solution with a concentration of 0.2 to 2% by weight. mineral acid. The concentration of mineral acids in the mother liquor is maintained within this range because the suspension of 2-methyl-4-chlorophenoxyacetic acid is well filterable within this range. Washing of the filter cake is not done because 2-methyl-4-chlorophenoxyacetic acid is soluble in water of 2 to 10 g / l (depending on temperature), which may cause product losses. In neutralizing the filter cake, the neutralizing agent, in addition to neutralizing 2-methyl-4-chlorophenoxyacetic acid, preferably neutralizes mineral acids, thereby causing its loss. This is disadvantageous especially when using more expensive neutralizing agents e.g. dimethylamine.
Vyššie uvedené nedostatky sú odstránené . zpósobom výroby dimetylamínovej soli 2-metyl4-chlórfenoxyoctovej kyseliny. Kyselina 2-metyl-4-chlórfenoxyoctová sa připraví chloráciou 2-metylfenoxyoctanu sodného s NaClO v přítomnosti minerálnej kyseliny. Zo získaného roztoku sa získá 2-metyl-4-chlórfenoxyoctová kyselina vyzrážanim v prebytočnej minerálnej kyselině.The above shortcomings are removed. by a process for preparing a dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid. 2-Methyl-4-chlorophenoxyacetic acid is prepared by chlorination of sodium 2-methylphenoxyacetate with NaClO in the presence of a mineral acid. The solution obtained is 2-methyl-4-chlorophenoxyacetic acid by precipitation in excess mineral acid.
Zo suspenzie sa vyzrážaná 2-metyl-4-chlórfenoxyoctová kyselina odfiltruje. Filtračný koláč obsahuje okrem 2-metyl-4-chlórfenoxyoctovej kyseliny aj matečný roztok minerálnych kyselin koncentrácii 0,2 až 2 % hmot. minerálnej kyseliny. Podstata vynálezu je v tom, že sa vo filtračnom koláči najskór neutralizujú minerálně kyseliny hydroxidmi, kysličníkmi, uhličitanmi alkalických kovov alebo alkalických zemin alebo amoniakom alebo uhličitanom amonným, připadne zmesou vyššie uvedených látok. Potom sa 2-metyl-4-chlórfenoxyoctová kyseliny zneutra lizuje dimetylamínom na dimetylaminovú sol 2-metyl-4-chlórfenoxyoctovej kyseliny.The precipitated 2-methyl-4-chlorophenoxyacetic acid is filtered from the suspension. In addition to 2-methyl-4-chlorophenoxyacetic acid, the filter cake also contains a mineral acid mother liquor concentration of 0.2 to 2% by weight. mineral acid. The essence of the invention is that in the filter cake the mineral acids are first neutralized with hydroxides, oxides, alkali metal or alkaline earth carbonates, or with ammonia or ammonium carbonate, optionally with a mixture of the aforementioned substances. Then, 2-methyl-4-chlorophenoxyacetic acid is neutralized with dimethylamine to the dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid.
Výhodou postupu podlá vynálezu je to, že sa použije na neutralizáciu minerálnych kyselin z filtračného koláča 2-metyl-4-chlórfenoxyoctovej kyseliny, lacnejšie neutralizačně činidlo ako dimetylamin, pričom sa výrobok zlační. Na herbicídnych vlastnostiach dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny sa nič nezmení. Prevedenie vynálezu je jednoduché dávkovanie sa dá robit na základe obsahu minerálnych kyselin vo filtráte po filtrácii 1-metyl-4-chlórfenoxyoctovej kyseliny.An advantage of the process according to the invention is that 2-methyl-4-chlorophenoxyacetic acid is used to neutralize mineral acids from the filter cake, a cheaper neutralizing agent than dimethylamine, whereby the product becomes glacial. Nothing changes on the herbicidal properties of the dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid. An embodiment of the invention is a simple dosage can be made based on the mineral acid content of the filtrate after filtration of 1-methyl-4-chlorophenoxyacetic acid.
Příklad 1Example 1
2-metyl-4-chlórfenoxyoctová kyselina sa připravila podlá čs. AO 179 200. Filtračný koláč obsahoval 42 % hmot. fenoxyoctových kyselin s obsahom 91,6 % hmot. 2-metyl-4-chlórfenoxyoctovej kyseliny a 1,8 % hmot. kyseliny chlorovodíkovéj. Najprv sa neutralizovala kyselina chlorovodíková ekvimolárnym množstvom 23 % hmot. amoniaku a potom sa zneutralizo- kovala 2-metyl-4-chlórfenoxyoctová kyselina s 40,6 % hmot. vodným roztokom dimetylamínu. Získaná dimetylamínová sol sa upravila přidáním vody na koncentráciu, pod ktorou sa předává ako výrobok (Aminex Pur). Po úpravě roztok obsahoval 28,5 % hmot. dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny i 0,2 % hmot. volného dimetylamínu.2-Methyl-4-chlorophenoxyacetic acid was prepared according to U.S. Pat. AO 179 200. The filter cake contained 42 wt. % phenoxyacetic acids with a content of 91.6% by weight; % Of 2-methyl-4-chlorophenoxyacetic acid and 1.8 wt. hydrochloric acid. First, the hydrochloric acid was neutralized with an equimolar amount of 23% by weight. % ammonia and then neutralizing 2-methyl-4-chlorophenoxyacetic acid with 40.6 wt. aqueous dimethylamine solution. The dimethylamine salt obtained was adjusted by adding water to a concentration below which it was passed as product (Aminex Pur). After treatment, the solution contained 28.5 wt. % dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid i 0.2 wt. of free dimethylamine.
Příklad 2Example 2
Postupovalo sa podlá příkladu 1 s tým rozdielom, že sa miesto amoniaku použil 10 % hmot. roztok KOH. Po úpravě roztok obsahoval 29,2 percent hmot. dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny a 0,4 % hmot. volného dimetylamínu.The procedure of Example 1 was followed except that 10 wt. KOH solution. After treatment, the solution contained 29.2 percent by weight. % dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid and 0.4 wt. of free dimethylamine.
Příklad 3Example 3
Postupovalo sa podlá příkladu 1 s tým rozdielom, že miesto amoniaku sa použil Mg(OH)2.The procedure of Example 1 was followed except that Mg (OH) 2 was used instead of ammonia.
Po úpravě roztok obsahoval 29,8 % dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny a neobsahoval volný dimetylamin.After treatment, the solution contained 29.8% dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid and did not contain free dimethylamine.
Příklad 4Example 4
Postupovalo sa podlá příkladu 1 s tým rozdielom, že sa miesto amoniaku použil 10-%ný roztok Na2COj. Po úpravě roztok obsahoval 28,2 percent dimetylamínovej soli 2-metyl-4-chlórfenoxyoctovej kyseliny a 0,1 % hmot. volného dimetylamínu.The procedure of Example 1 was followed except that a 10% Na 2 CO 3 solution was used instead of ammonia. After treatment, the solution contained 28.2 percent of 2-methyl-4-chlorophenoxyacetic acid dimethylamine salt and 0.1 wt. of free dimethylamine.
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| CS845976A CS265751B1 (en) | 1984-08-06 | 1984-08-06 | Method of 2-methyl-4-chlorphenoxy acetic acid's dimethylamine salt production |
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| CS845976A CS265751B1 (en) | 1984-08-06 | 1984-08-06 | Method of 2-methyl-4-chlorphenoxy acetic acid's dimethylamine salt production |
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| CS597684A1 CS597684A1 (en) | 1989-03-14 |
| CS265751B1 true CS265751B1 (en) | 1989-11-14 |
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