CS225558B1 - Manufacture of mucochlorine acid of the chemical standard purity - Google Patents
Manufacture of mucochlorine acid of the chemical standard purity Download PDFInfo
- Publication number
- CS225558B1 CS225558B1 CS814481A CS814481A CS225558B1 CS 225558 B1 CS225558 B1 CS 225558B1 CS 814481 A CS814481 A CS 814481A CS 814481 A CS814481 A CS 814481A CS 225558 B1 CS225558 B1 CS 225558B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- acid
- mucochloric acid
- purity
- chemical standard
- mucochloric
- Prior art date
Links
- 239000000126 substance Substances 0.000 title claims description 9
- 239000002253 acid Substances 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title description 4
- LUMLZKVIXLWTCI-NSCUHMNNSA-N (e)-2,3-dichloro-4-oxobut-2-enoic acid Chemical compound OC(=O)C(\Cl)=C(/Cl)C=O LUMLZKVIXLWTCI-NSCUHMNNSA-N 0.000 claims description 31
- ZAKLKBFCSHJIRI-UHFFFAOYSA-N mucochloric acid Natural products OC1OC(=O)C(Cl)=C1Cl ZAKLKBFCSHJIRI-UHFFFAOYSA-N 0.000 claims description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims 1
- 229940005991 chloric acid Drugs 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 241000219310 Beta vulgaris subsp. vulgaris Species 0.000 description 1
- 235000021536 Sugar beet Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Vynálezom je spósob výroby kyseliny raukochlórovej vzorcaThe present invention is a process for the preparation of rucochloric acid of the formula
CiC
C — COHC - COH
C — COOHC-COOH
Cl čistoty chemického standardu kryštalizáciou z vodného roztoku za použitia aktívneho uhlia s možnosťou recyklácie filtrátu.Cl of the chemical standard purity by crystallization from an aqueous solution using activated carbon with the possibility of recycling the filtrate.
Technická kyselina mukochlórová sa získává různým výrobným postupom napr. chloráciou furalu v prostředí matečného roztoku, alebo v prostředí kyseliny chlorovodíkové] zvyčajne chloráciou pri teplotách 60 až 80 °C.Technical mucochloric acid is obtained by various production processes, e.g. by chlorination of the fural in the mother liquor or in the hydrochloric acid medium] usually by chlorination at temperatures of 60 to 80 ° C.
Kyselina mukochlórová je důležitým východzím produktom pri výrobě různých organických výrobkov, například pri výrobě selektívnych herbicídov do cukrovej řepy.Mucochloric acid is an important starting product in the production of various organic products, for example, in the production of selective sugar beet herbicides.
Technická kyselina mukochlórová, vyrobená chloráciou furalu v prostředí vratného a upraveného matečného roztoku, alebo v prostředí kyseliny chlorovodíkové] je spravidla 96 a 98 % čistoty. Nečistotami sú sprievodné látky vznikajúce v procese chlorácle furalu.The technical mucochloric acid produced by the chlorination of fural in a returning and treated mother liquor environment or in a hydrochloric acid environment] is generally 96 and 98% pure. The impurities are the accompanying substances produced in the fural chlorate process.
Doposial' zaužívané postupy výrob neuvažujú s dodatočným čistěním.The processes of the prior art do not provide for additional purification.
Autoři S. Beattie, I. M. Heilbren a F. Irving (Soc. Chem. 1932) čistia kyselinu mukochlórová premytím vodnoalkoholickým roztokom, čím sa zbavuje reakčného filtrátu.S. Beattie, I M. Heilbren, and F. Irving (Soc. Chem. 1932) purify mucochloric acid by washing with a water-alcoholic solution to remove the reaction filtrate.
Podstata vynálezu spočívá v tom, že technická kyselinu mukochlórová získaná spůsobom uvedeným v úvode možno čistiť procesoru kryštalizácie z vodného roztoku za použitia aktívneho uhlia, pričom sa získá kyselina mukochlórová vysokej čistoty.SUMMARY OF THE INVENTION The technical mucochloric acid obtained by the above process can be purified by crystallization from an aqueous solution using activated carbon to obtain high purity mucochloric acid.
Podl'a predmetu vynálezu sa vyrába kyselina mukochlórová, čistoty chemického standardu tak, že sa technická kyselina mukochlórová rozpustí za mlešania v horúcej vodě o teplote 50 až 80 °C. Množstvo technickej kyseliny mukochlórovej je 5 až 60 g na 100 g vody, s výhodou sa pracuje s koncentráciou 15 až 20 g na 100 g vody. Horáci roztok sa nechá ochladit na teplotu 5 až 20 °C a izoluje sa vykrystalizovaná kyselina mukochlórová z matečného roztoku. Takto získaná kyselina mukochlórová sa opatovne rozpustí vo vodě na roztok obsahujúci 5 až .60 g kyseliny na 100 g vody, s výhodou 15 až 20 g na 100 g vody pri teplote maximálně 80 °C, pričom sa do roztoku přidá za miešania účelne 0,5 až 1,0 g aktívneho uhlia. Aktivně uhlie možno pridať v množstve maximálně 5 % hmot., vztahované oddělí od roztoku kyseliny mukochlórovej, roztok sa ochladí na teplotu + 5 až 20 °C a vykrystalizovaná kyselina mukochlórová sa oddělí od matečného roztoku filtráciou, ďalej sa premyje malým množstvom vody a vysuší sa.According to the present invention, mucochloric acid of chemical standard purity is produced by dissolving technical mucochloric acid with stirring in hot water at a temperature of 50 to 80 ° C. The amount of technical mucochloric acid is 5 to 60 g per 100 g of water, preferably a concentration of 15 to 20 g per 100 g of water is used. The hot solution was allowed to cool to 5 to 20 ° C and crystallized mucochloric acid was isolated from the mother liquor. The mucochloric acid thus obtained is carefully dissolved in water to a solution containing 5 to 60 g of acid per 100 g of water, preferably 15 to 20 g per 100 g of water at a temperature of not more than 80 ° C, preferably 0, 5 to 1.0 g of activated carbon. Activated charcoal may be added at a maximum of 5% by weight, separated from the mucochloric acid solution, the solution is cooled to + 5 to 20 ° C and the crystallized mucochloric acid is separated from the mother liquor by filtration, further washed with a small amount of water and dried .
Proces kryštalizácie možno niekotkokrát opakovat. Mdže byť uskutočnený aj bez pridávania aktívneho uhlia v závislosti od čistoty technickej kyseliny mukochlórovej použitej na čistenie.The crystallization process can be repeated several times. It can also be carried out without the addition of activated carbon, depending on the purity of the technical mucochloric acid used for the purification.
Postup je vyznačený tým, že sa aspoň jedenkrát opakuje rozpustenie, chladenie a izolácia, po případe za přídavku aktívneho uhlia.The process is characterized in that the dissolution, cooling and isolation are repeated at least once, optionally with the addition of activated carbon.
Po opakovanej kryštalizácii sa získává kyselina mukochlórová vysokej čistoty, zodpovedajúcej čistotě chemického standardu.After repeated crystallization, mucochloric acid of high purity, corresponding to the purity of the chemical standard, is obtained.
Na prvý stupeň rozpúšťania technickej kyseliny mukochlórovej možno použit filtrát získaný z kryštalizácie produktu.The filtrate obtained from crystallization of the product can be used for the first stage of dissolution of industrial mucochloric acid.
Predmet vynálezu možno použit při přípravě kyseliny mukochlórovej čistoty chemického Standardu.The present invention can be used in the preparation of mucochloric acid of the chemical standard purity.
Predmety vynálezu dokumentujú příklady, ktoré však nevyčerpávajú rozsah uplatnenia.The objects of the invention illustrate examples which, however, do not exhaust the scope of application.
Příklad 1Example 1
150 g technickej kyseliny mukochlórovej sa rozpustilo za miešania v 1000 ml vody, pričom teplota roztoku nepresiahla 80 °C. Po ochladení roztoku sa vykrystalizovaná kyselina mukochlórová odfiltrovala na Buchnerovom lieviku a podrobila sa druhej kryštalizácii v 1000 ml vody pri maximálnej teplote 80 °C, pričom sa přidalo za miešania 5 g aktívneho uhlia. Horúci roztok sa po 15 minutách miešania přefiltroval, ochladil na 20 °C a vypadnuté kryštály mukochlórovej kyseliny sa premyli so 100 ml studenej vody. Po vysušení sa získalo 108 g kyseliny mukochlórovej s teplotou topenia 126,8 °C.150 g of technical mucochloric acid were dissolved with stirring in 1000 ml of water, the temperature of the solution not exceeding 80 ° C. After cooling the solution, the crystallized mucochloric acid was filtered off on a Buchner funnel and subjected to a second crystallization in 1000 ml of water at a maximum temperature of 80 ° C, while adding 5 g of activated carbon with stirring. After stirring for 15 minutes, the hot solution was filtered, cooled to 20 ° C and the precipitated mucochloric acid crystals were washed with 100 ml of cold water. After drying, 108 g of mucochloric acid with a melting point of 126.8 ° C were obtained.
Příklad 2Example 2
Postupovalo sa ako v příklade 1, s tým rozdielom, že sa previedli 3 kryštalizácie bez použitia aktívneho uhlia. Získalo sa 91 g mukochlórovej kyseliny s teplotou topeniaThe procedure was as in Example 1, except that 3 crystallizations were carried out without the use of activated carbon. 91 g of mucochloric acid having a melting point was obtained
126.7 °C.126.7 ° C.
Příklad 3Example 3
Postupovalo sa ako v příklade 1, pričom sa na rozpustenie technickej kyseliny mukochlórovej použilo 1000 ml filtrátu, získaného po poslednej filtrácii kyseliny mukochlórovej v příklade 1. Získaný produkt — kyselina mukochlórová — mala teplotu topeniaThe procedure was as in Example 1, wherein 1000 ml of the filtrate obtained after the last filtration of mucochloric acid in Example 1 was used to dissolve the technical mucochloric acid.
126.8 °C.126.8 ° C.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS814481A CS225558B1 (en) | 1981-11-05 | 1981-11-05 | Manufacture of mucochlorine acid of the chemical standard purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS814481A CS225558B1 (en) | 1981-11-05 | 1981-11-05 | Manufacture of mucochlorine acid of the chemical standard purity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS225558B1 true CS225558B1 (en) | 1984-02-13 |
Family
ID=5431627
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS814481A CS225558B1 (en) | 1981-11-05 | 1981-11-05 | Manufacture of mucochlorine acid of the chemical standard purity |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS225558B1 (en) |
-
1981
- 1981-11-05 CS CS814481A patent/CS225558B1/en unknown
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