SU438653A1 - The method of decontamination waste production lithium alkyls - Google Patents
The method of decontamination waste production lithium alkylsInfo
- Publication number
- SU438653A1 SU438653A1 SU1858221A SU1858221A SU438653A1 SU 438653 A1 SU438653 A1 SU 438653A1 SU 1858221 A SU1858221 A SU 1858221A SU 1858221 A SU1858221 A SU 1858221A SU 438653 A1 SU438653 A1 SU 438653A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- lithium
- chloride
- waste production
- decontamination waste
- lithium alkyls
- Prior art date
Links
- 229910052744 lithium Inorganic materials 0.000 title description 20
- 238000000034 method Methods 0.000 title description 12
- 239000002699 waste material Substances 0.000 title description 8
- 238000005202 decontamination Methods 0.000 title description 5
- 230000003588 decontaminative effect Effects 0.000 title description 3
- 238000004519 manufacturing process Methods 0.000 title description 3
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 14
- -1 lithium halide Chemical class 0.000 description 7
- 239000010802 sludge Substances 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 150000001350 alkyl halides Chemical class 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical compound [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 150000002900 organolithium compounds Chemical class 0.000 description 1
- 125000001979 organolithium group Chemical group 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Processing Of Solid Wastes (AREA)
Description
1one
Изобретение касаетс улучшени способа дезактивации отходов нрОИвводства литийалкилов , которые наход т широкое применение в химическом rap омышленном синтезе.The invention relates to the improvement of the method of decontamination of waste production of lithium alkyls, which are widely used in chemical and industrial synthesis.
Литийалкилы получают из металлического лити и галоидного алкила. Образующиес отходы (шлам) представл ют собой смесь галоидного лити с непрореагировавшим металлическим литием и остатками литийорганического соединени . В св зи с тем, что синтез литийаЛКилов провод т обычно с применением избытка металла, содержание последнего в шламе может достигать 1 % и более. Наличие металлического лити в виде тонкой дисперсии и литийорганического соединени придают шламу значительную пирофорность, приближающуюс к пирофорности цези .Lithium alkyls are derived from lithium metal and alkyl halide. The resulting waste (sludge) is a mixture of lithium halide with unreacted lithium metal and residues of organolithium. Since lithium-LKyls are usually synthesized using an excess of metal, the content of the latter in the sludge can reach 1% or more. The presence of metallic lithium in the form of a fine dispersion and organolithium compound gives the sludge a significant pyrophoricity approaching that of cesium.
Известен способ дезактивации отходов ще .точных металлов с использованием в качестве дезактивирующего вещества пепообразовател ПО-1, который состоит из 5-8 вес. ч. 50%ного водного раствора очищенного«еросииового контакта, 3-5 вес. ч. 28%-ного водного раствора стол рного кле и 1 вес. ч. спиртасырца . По такому способу металл (литий) можно получить только в виде гидроокиси, «которую затем нео1бходимо превратить в хлорид лити действием хлора, хлористого водорода или сол ной кислоты, поскольку хлорид лити вл етс пока единственным соединением , из которого металлический литий получают электролизом в промышленном масштабе . Кроме того, в процесс дезактивации с помощью ПО-1 .выдел етс значительное количество водорода, что делает процесс небезопасным .There is a known method for the decontamination of waste metals of the exact metals using the PO-1 as a deactivating agent, which consists of 5-8 wt. including a 50% strength aqueous solution of purified “erosine contact, 3-5 wt. including 28% aqueous solution of table glue and 1 wt. h alcohols. By this method, metal (lithium) can only be obtained in the form of hydroxide, "which then must be converted into lithium chloride by the action of chlorine, hydrogen chloride or hydrochloric acid, since lithium chloride is still the only compound from which metallic lithium is produced by electrolysis on an industrial scale. . In addition, significant amount of hydrogen is released in the decontamination process with PO-1, which makes the process unsafe.
Целью изобретени вл етс упрощение процесса дезактивации.The aim of the invention is to simplify the decontamination process.
Эта цель достигаетс обработкой углеводородной суспензии отходов галоидным алкилом с последующим растворением образующегос галогенида лити в воде и выделением его известными приемами.This goal is achieved by treating the waste hydrocarbon suspension with alkyl halide followed by dissolving the lithium halide that forms in water and isolating it with known techniques.
Предлагаемый способ заключаетс в том, что шлам после отделени от раствора литийалкила в среде углеводорода обрабатывают галоидным алкилом, преимущественно при 20-100°С, с целью перевода металлического лити в галоидный литий и образовавшегос литийаЛКила в галогенид лити и углеводород . Полученный галогенид лити раствор ют в воде с последующим выделением его известными приемами.The proposed method consists in that the sludge, after being separated from the solution of lithium alkyl in the hydrocarbon medium, is treated with alkyl halide, preferably at 20-100 ° C, to convert lithium metal to lithium halide and the lithium lithium formed in lithium halide and hydrocarbon. The resulting lithium halide is dissolved in water, followed by separation by known techniques.
Пример 1. В аппарат емкостью 200 л загружают 80 л суспензии шлама в бензине (растворитель дл полиэтилена низкого давлени ), котора состоит из 70 л бензина и 10 кг шлама, содержащего 9,76 кг хлорида лити , 0,14 кг свободного металлического лити и 0,3 л бутиллити . Затем при работающей мешалке в аппарат подают 4,4 л хлористого н-бутила, смесь нагревают до 70°С и выдерживают при этой температуре в течение 8 час. В результате реакции весь металлический литий превращаетс в хлорид, а бутиллитий - в октан и хлорид лити . 9,9 КГ суспензии хлорида в углеводородном растворителе подают в аппарат емкостью 200 л, снабженный мешалкой и охладительной рубашкой, в который предварительно наливают 100 л воды. Растворение хлорида лити сопровождаетс выделением водорода (12 л на 1 «г вз того шлама) вследствие выш;елачивани водой лити , вошедшего в кристаллическую решетку хлорида. Полученный раство-р нейтрализуют разбавленной сол ной кислотой до рН 6, водный слой отдел ют , упаривают и выдел ют хлорид лити в виде мойогидрата. Органической слой очищают известными методами и возвращают в рецикл.Example 1. A 200 l apparatus is charged with 80 l of slurry suspension in gasoline (solvent for low pressure polyethylene), which consists of 70 l of gasoline and 10 kg of sludge containing 9.76 kg of lithium chloride, 0.14 kg of free lithium metal and 0.3 liter utility. Then, with the mixer running, 4.4 liters of n-butyl chloride are fed into the apparatus, the mixture is heated to 70 ° C and maintained at this temperature for 8 hours. As a result of the reaction, all metallic lithium is converted to chloride, and butyl lithium to octane and lithium chloride. 9.9 KG of chloride suspension in a hydrocarbon solvent is fed to an apparatus with a capacity of 200 liters, equipped with a stirrer and a cooling jacket, into which 100 liters of water are pre-poured. The dissolution of lithium chloride is accompanied by the release of hydrogen (12 liters per 1 "g of sludge) as a result of elevation; leaching of lithium with water, which entered the crystal lattice of chloride. The resulting solution is neutralized with dilute hydrochloric acid to pH 6, the aqueous layer is separated, evaporated and lithium chloride is recovered as myohydrate. The organic layer is purified by known methods and returned to recycling.
Результаты анализа щелевого Продукта в сравнении с техническим ЦМТУ 3043-51 приведены в таблице.The results of the analysis of the slit Product in comparison with the technical CMTU 3043-51 are given in the table.
Как видно из данных таблицы, оолученный из отходов хлорид лити удовлетвор ет техническим услови м.As can be seen from the data in the table, lithium chloride obtained from waste meets the technical conditions.
Предмет изобретени Subject invention
Способ дезактивации отходов производства литийалкилов путем обработки дезактивирующим веществом, отличающийс тем, что, с целью упрощени процесса, углеводородную суспензию отходов обрабатывают галоидным алкилом с последующим растворением образующегос галогенида лити в воде и выделением его известными приемами.A method for deactivating waste production of lithium alkyls by treating with a deactivating agent, characterized in that, in order to simplify the process, the hydrocarbon suspension of the waste is treated with alkyl halide followed by dissolving the lithium halide formed in water and isolating it with known techniques.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1858221A SU438653A1 (en) | 1972-12-14 | 1972-12-14 | The method of decontamination waste production lithium alkyls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1858221A SU438653A1 (en) | 1972-12-14 | 1972-12-14 | The method of decontamination waste production lithium alkyls |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU438653A1 true SU438653A1 (en) | 1974-08-05 |
Family
ID=20535366
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU1858221A SU438653A1 (en) | 1972-12-14 | 1972-12-14 | The method of decontamination waste production lithium alkyls |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU438653A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326640C (en) * | 2004-10-01 | 2007-07-18 | 中国石化集团巴陵石油化工有限责任公司 | Hydrolysis method for lithium slag from lithium alkyl synthesis |
-
1972
- 1972-12-14 SU SU1858221A patent/SU438653A1/en active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326640C (en) * | 2004-10-01 | 2007-07-18 | 中国石化集团巴陵石油化工有限责任公司 | Hydrolysis method for lithium slag from lithium alkyl synthesis |
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