SU322322A1 - METHOD OF CLEANING XYLILENEDIAMINES - Google Patents
METHOD OF CLEANING XYLILENEDIAMINESInfo
- Publication number
- SU322322A1 SU322322A1 SU1212535A SU1212535A SU322322A1 SU 322322 A1 SU322322 A1 SU 322322A1 SU 1212535 A SU1212535 A SU 1212535A SU 1212535 A SU1212535 A SU 1212535A SU 322322 A1 SU322322 A1 SU 322322A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- weight
- xylylenediamine
- cleaning
- water
- xylilenediamines
- Prior art date
Links
- 238000004140 cleaning Methods 0.000 title description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- GKXVJHDEWHKBFH-UHFFFAOYSA-N [2-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC=C1CN GKXVJHDEWHKBFH-UHFFFAOYSA-N 0.000 description 6
- LAQPNDIUHRHNCV-UHFFFAOYSA-N isophthalonitrile Chemical compound N#CC1=CC=CC(C#N)=C1 LAQPNDIUHRHNCV-UHFFFAOYSA-N 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 125000005219 aminonitrile group Chemical group 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 150000004985 diamines Chemical class 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- XFKPORAVEUOIRF-UHFFFAOYSA-N 3-(aminomethyl)benzonitrile Chemical compound NCC1=CC=CC(C#N)=C1 XFKPORAVEUOIRF-UHFFFAOYSA-N 0.000 description 1
- XQZYPMVTSDWCCE-UHFFFAOYSA-N Phthalonitrile Chemical compound N#CC1=CC=CC=C1C#N XQZYPMVTSDWCCE-UHFFFAOYSA-N 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- BHXFKXOIODIUJO-UHFFFAOYSA-N benzene-1,4-dicarbonitrile Chemical compound N#CC1=CC=C(C#N)C=C1 BHXFKXOIODIUJO-UHFFFAOYSA-N 0.000 description 1
- 125000000879 imine group Chemical group 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 150000003022 phthalic acids Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Description
Известен способ очистки ксилилендиаминов путем экстракции примесей из ксилилендиаминов в системе жидкость - жидкость насыщенными алифатическими, циклоалифатическими или ароматическими углеводородами.A known method of purification of xylylenediamine by extracting impurities from xylylenediamine in the system liquid - liquid saturated aliphatic, cycloaliphatic or aromatic hydrocarbons.
С целью упрощени процесса, предлагаетс способ очистки ксилилендиаминов, полученных при гидрировании динитрилов фталевых кислот, от примесей, содержащих нитрильную , иминную или амидную группы, заключающийс в том, что очистку осуществл ют путем гидролиза при температуре до 200°С. Гидролиз желательно проводить в присутствии оснований, например щелочи или аммиака .In order to simplify the process, a method is proposed for purifying xylylenediamines obtained by hydrogenating dinitriles with phthalic acids from impurities containing nitrile, imine or amide groups, which consists in cleaning by hydrolysis at temperatures up to 200 ° C. The hydrolysis is preferably carried out in the presence of bases, for example alkali or ammonia.
Пример 1. К 50 вес. ч. лг-ксилилендиамина , содержащего 2,0 вес. %. 3-цианбензиламина и 1,0 вес. % изофталопитрила, добавл ют 50 вес. ч. 1%-ного водного раствора NaOH. Воду отгон ют, затем перегон ют ксилилендиамип . В полученном образце цианбензиламина и изофталонитрила не обнаруживают.Example 1. To 50 wt. including lg-xylylenediamine containing 2.0 weight. % 3-cyanbenzylamine and 1.0 weight. % isophthalopitrile, add 50 weight. including 1% aqueous solution of NaOH. The water is distilled off, then the xylylenediamine is distilled. Cyanbenzylamine and isophthalonitrile are not detected in the obtained sample.
Пример 2. К 50 вес. ч. ж-ксилилендиамина , содержащего 1,5 вес. % изофталонитрила, добавл ют 50 вес. ч. водного аммиака, затем воду и аммиак 01гон ют и перегонкой диамина получают образец, не содержащий изо-, фталонитрила.Example 2. To 50 wt. h, xylylenediamine containing 1.5 weight. % isophthalonitrile, add 50 weight. including aqueous ammonia, then water and ammonia, and distillation of the diamine gives a sample that does not contain iso-, phthalonitrile.
н ют и перегонкой диамина под вакуумом получают образец, не содержащий изофталонитрила .A sample without isophthalonitrile is obtained by distilling the diamine under vacuum.
Пример 4. К 50 вес. ч. лг-ксилилендиамина , содерл ащего 2,0 вес. % изофталонитрила и 2,0 вес. % аминонитрила, добавл ют 50 вес. ч. воды и смесь греют при давлении 10 аг и в течение 6 час. Затем отгон ют воду, диамин перегон ют под вакуумомExample 4. To 50 wt. h lg-xylylenediamine, containing 2.0 weight. % isophthalonitrile and 2.0 weight. % aminonitrile, add 50 weight. including water and the mixture is heated at a pressure of 10 arg and for 6 hours. Then water is distilled off, the diamine is distilled under vacuum.
и получают образец, не содержащий изофталонитрила и аминонитрила.and get a sample that does not contain isophthalonitrile and aminonitrile.
Пример 5. К 50 вес. ч. лг-ксилилендиамина , содержащего 2,0 вес. % терефталонитрила и 2,0 вес. % «-аминонитрила, добавл ютExample 5. To 50 wt. including lg-xylylenediamine containing 2.0 weight. % terephthalonitrile and 2.0 weight. % "-Aminonitrile added
50 вес. ч. 1,5%-ного раствора щелочи. Воду отгон ют и после перегонки под вакуумом получают п-ксилилендиамин, не содержащий примесей динитрила и аминонитрила.50 wt. including 1.5% alkaline solution. The water is distilled off and, after distillation under vacuum, p-xylylenediamine is obtained, which does not contain impurities of dinitrile and aminonitrile.
Пример 6. К 50 вес. ч. л«-ксилилендиамипа , содержащего 1 вес. % изофталонитрила, добавл ют 50 вес. ч. воды. Смесь нагревают до 70°С и выдерживают при этой температуре 6 час, после чего анализ смеси указывает на отсутствие динитрила. После отгонки водыExample 6. To 50 wt. hours l "-xylanediamine containing 1 wt. % isophthalonitrile, add 50 weight. h of water. The mixture is heated to 70 ° C and maintained at this temperature for 6 hours, after which the analysis of the mixture indicates the absence of dinitrile. After the distillation of water
получают ксилилендиамин, не содержащий дипитрила.get xylylenediamine, not containing dipitrile.
Предмет изобретени 34The subject invention 34
с целью упрощени процесса, очистку прово-2. Способ по п. 1, отличающийс тем, чтоin order to simplify the process, cleaning wire-2. A method according to claim 1, characterized in that
д т-путем гидролиза при температуре до гидролиз провод т в присутствии оснований. 200°С.например щелочи или аммиака.dt-by hydrolysis at a temperature before the hydrolysis is carried out in the presence of bases. 200 ° C. For example, alkali or ammonia.
322322 322322
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU322322A1 true SU322322A1 (en) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8142618B2 (en) | 2006-02-01 | 2012-03-27 | Basf Aktiengesellschaft | Processes for preparing pure xylylenediamine |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8142618B2 (en) | 2006-02-01 | 2012-03-27 | Basf Aktiengesellschaft | Processes for preparing pure xylylenediamine |
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