BE357252A - - Google Patents
Info
- Publication number
- BE357252A BE357252A BE357252DA BE357252A BE 357252 A BE357252 A BE 357252A BE 357252D A BE357252D A BE 357252DA BE 357252 A BE357252 A BE 357252A
- Authority
- BE
- Belgium
- Prior art keywords
- chlorination
- waxy
- catalysts
- chlorine content
- temperature
- Prior art date
Links
- 238000005660 chlorination reaction Methods 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- 150000002790 naphthalenes Chemical class 0.000 claims description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 241000207199 Citrus Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/14—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the side-chain of aromatic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
<Desc/Clms Page number 1>
Procédé d'obtention de naphtalines chlorées de nature ci- reuse*
On a cherché différentes reprises à fabriquer des masses cireuses de naphtaline par chloration. D' après le brevet américain N0 914,223 du 2 mars 1909 on peut obtenir, en poussant assez loin la chloration de naphta- line, à des températures supérieures et sous pression,
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des masses solides cireuses qui ont une teneur en chlore de 68% environ, c'est-à-dire de 7 à 8 atomes de chlore dans la molécule. On peut alors opérer aussi en présence de catalyseurs.
Si lon veut fabriquer de tels produits cireux à une teneur en chlore de moins de 60 %,-de 50 à 57% exemple,- on est obligé, diaprés les indications du Brevet Allemand ? 319.253 du 21 octobre 1916 d'éviter la pré- sence de métaux, tels que: fer, antimoine et autres, parce que ceux-ci, à titre de catalyseurs pour matières à action chlorante, exercent une influence extrêmement défavorable sur la nature cireuse voulue du produit final. Pour la réalisation de la chloration, la tempéra- ture monte au cours de l'opération à la valeur de 150 à 170 G., bien que l'opération exige plusieurs jours.
Or on fait l'observation surprenante que l'on peut arriver à obtenir, en un temps sensiblement plus court, des masses précieuses de nature cireuse à une teneur en chlore au -dessous de 60%, si l'on opère la chloration en présence de catalyseurs, tels que par exemple: anti- moine, phosphore, soufre, iode, et leurs composés, et si l'on maintient alors la température au-dessous de 130 C.
On fait cesser la chloration dès qu'on constate la con- sistance voulue sur une prise dressai que 1'fin a laissé refroidir.
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Exemples
A un mélange de 2.000 parties de naphtaline,, on ajoute 20 parties de trichlorure d'antimoine et on porte la masse à la fusion. Dans l'espace de 10 heures; 4.400 parties de chlore sont introduites, la température étant maintenue si basse-que la masse est encore mobile. La masse fondue est soufflée quelque temps encore avec de l'air et elle peut être employée directement. ou bien dis- tillée à pression réduite. Si l'on maintient plus éle- vée dès le début la température dans ltexemple, sans dépasser néanmoins 130 C.,le point d'écoulement en goutte de la masse terminée monte d"environ 100 C. à 120 C.
<Desc / Clms Page number 1>
Process for obtaining chlorinated naphthalene of a citrus nature *
Various attempts have been made to manufacture waxy masses of naphthalene by chlorination. According to US Pat. No. 914,223 of March 2, 1909, it is possible to obtain, by pushing the chlorination of naphthalin far enough, at higher temperatures and under pressure,
<Desc / Clms Page number 2>
waxy solids which have a chlorine content of about 68%, that is to say from 7 to 8 chlorine atoms in the molecule. It is then possible to operate also in the presence of catalysts.
If one wants to manufacture such waxy products with a chlorine content of less than 60%, - from 50 to 57% for example, - one is obliged, according to the indications of the German patent? 319.253 of October 21, 1916 to avoid the presence of metals, such as: iron, antimony and others, because these, as catalysts for substances with chlorinating action, exert an extremely unfavorable influence on the desired waxy nature of the final product. For carrying out the chlorination, the temperature rises during the operation to the value of 150 to 170 G., although the operation requires several days.
Now, we make the surprising observation that it is possible to obtain, in a significantly shorter time, precious masses of a waxy nature at a chlorine content below 60%, if the chlorination is carried out in the presence of catalysts, such as, for example: anti-monk, phosphorus, sulfur, iodine, and their compounds, and if the temperature is then maintained below 130 C.
The chlorination is stopped as soon as the desired consistency is observed on an upright set which has been left to cool.
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Examples
To a mixture of 2,000 parts of naphthalene, 20 parts of antimony trichloride are added and the mass is brought to fusion. Within 10 hours; 4,400 parts of chlorine are introduced, the temperature being kept so low that the mass is still mobile. The melt is blown for some time with air and can be used directly. or else distilled at reduced pressure. If the temperature in the example is kept higher from the start, but without exceeding 130 ° C., the drop pour point of the finished mass rises from about 100 ° C. to 120 C.
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| BE357252A true BE357252A (en) |
Family
ID=31167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| BE357252D BE357252A (en) |
Country Status (1)
| Country | Link |
|---|---|
| BE (1) | BE357252A (en) |
-
0
- BE BE357252D patent/BE357252A/fr unknown
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