DE2531925A1 - Verfahren zur herstellung eines basisdetergents fuer fluessige waschmittel - Google Patents
Verfahren zur herstellung eines basisdetergents fuer fluessige waschmittelInfo
- Publication number
- DE2531925A1 DE2531925A1 DE19752531925 DE2531925A DE2531925A1 DE 2531925 A1 DE2531925 A1 DE 2531925A1 DE 19752531925 DE19752531925 DE 19752531925 DE 2531925 A DE2531925 A DE 2531925A DE 2531925 A1 DE2531925 A1 DE 2531925A1
- Authority
- DE
- Germany
- Prior art keywords
- acid
- detergent
- aliphatic
- ammonia
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000003599 detergent Substances 0.000 title claims description 24
- 239000007788 liquid Substances 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 16
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 12
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 8
- 239000001361 adipic acid Substances 0.000 claims description 8
- 235000011037 adipic acid Nutrition 0.000 claims description 8
- -1 aliphatic amines Chemical class 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 150000001414 amino alcohols Chemical class 0.000 claims description 4
- 239000000787 lecithin Substances 0.000 claims description 4
- 229940067606 lecithin Drugs 0.000 claims description 4
- 235000010445 lecithin Nutrition 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 2
- 150000002830 nitrogen compounds Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 239000003925 fat Substances 0.000 description 5
- 235000019197 fats Nutrition 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 241001494246 Daphnia magna Species 0.000 description 4
- 230000001236 detergent effect Effects 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000004310 lactic acid Substances 0.000 description 3
- 235000014655 lactic acid Nutrition 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 239000001741 Ammonium adipate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 235000019293 ammonium adipate Nutrition 0.000 description 2
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 2
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 150000004665 fatty acids Chemical group 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 2
- 235000019871 vegetable fat Nutrition 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 1
- 208000035859 Drug effect increased Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000008431 aliphatic amides Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000010763 heavy fuel oil Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 229940116351 sebacate Drugs 0.000 description 1
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
- C02F1/682—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water by addition of chemical compounds for dispersing an oily layer on water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/002—Non alkali-metal soaps
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Microbiology (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7425834A FR2283218A1 (fr) | 1974-07-25 | 1974-07-25 | Detergent de base pour lessives liquides |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE2531925A1 true DE2531925A1 (de) | 1976-02-05 |
Family
ID=9141689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19752531925 Withdrawn DE2531925A1 (de) | 1974-07-25 | 1975-07-17 | Verfahren zur herstellung eines basisdetergents fuer fluessige waschmittel |
Country Status (26)
| Country | Link |
|---|---|
| US (1) | US3996148A (en, 2012) |
| JP (1) | JPS5137103A (en, 2012) |
| AR (1) | AR206539A1 (en, 2012) |
| AT (1) | AT343250B (en, 2012) |
| AU (1) | AU8337275A (en, 2012) |
| BE (1) | BE831740A (en, 2012) |
| BR (1) | BR7504780A (en, 2012) |
| CA (1) | CA1079747A (en, 2012) |
| CH (1) | CH597341A5 (en, 2012) |
| DD (1) | DD122824A5 (en, 2012) |
| DE (1) | DE2531925A1 (en, 2012) |
| DK (1) | DK338675A (en, 2012) |
| ES (1) | ES439717A1 (en, 2012) |
| FI (1) | FI752136A7 (en, 2012) |
| FR (1) | FR2283218A1 (en, 2012) |
| GB (1) | GB1521984A (en, 2012) |
| IE (1) | IE41641B1 (en, 2012) |
| IL (1) | IL47748A (en, 2012) |
| IN (1) | IN144017B (en, 2012) |
| IT (1) | IT1040009B (en, 2012) |
| LU (1) | LU73054A1 (en, 2012) |
| NL (1) | NL7508887A (en, 2012) |
| NO (1) | NO752595L (en, 2012) |
| OA (1) | OA05062A (en, 2012) |
| SE (1) | SE7508420L (en, 2012) |
| ZA (1) | ZA754801B (en, 2012) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0008060A1 (de) * | 1978-08-03 | 1980-02-20 | BASF Aktiengesellschaft | Verwendung von mehrwertigen Alkoholen, (Hydroxy)carbonsäuren und/oder deren Estern mit den mehrwertigen Alkoholen als Viskositätsregler |
| EP0213475A3 (en) * | 1985-08-24 | 1988-01-13 | Bayer Ag | Polyesterpolyols, process for their fabrication and their utilisation in the isocyanate-polyaddition process |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4250042A (en) * | 1979-04-16 | 1981-02-10 | The Lubrizol Corporation | Corrosion inhibition in well-drilling operations using aqueous systems containing ammonium carboxylates |
| JPS5637252A (en) * | 1979-08-30 | 1981-04-10 | Sekisui Chem Co Ltd | Interlayer for laminated glass |
| US20080026974A1 (en) * | 2006-07-27 | 2008-01-31 | Barnhart Ronald A | Antimicrobial hand wash |
| GB201615047D0 (en) * | 2016-09-05 | 2016-10-19 | Spheritech Ltd | Microparticle composition and use thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2691636A (en) * | 1954-10-12 | naoocchs | ||
| US3072502A (en) * | 1961-02-14 | 1963-01-08 | Pfizer & Co C | Process for removing copper-containing iron oxide scale from metal surfaces |
| US3166444A (en) * | 1962-04-26 | 1965-01-19 | Lubrizol Corp | Method for cleaning metal articles |
| US3554801A (en) * | 1969-12-03 | 1971-01-12 | Ethyl Corp | Method of removing manganese oxide deposits |
| US3661787A (en) * | 1970-10-09 | 1972-05-09 | Pollutrol Group The | Saturated aliphatic dicarboxylic acid salts as detergent builders |
| US3703481A (en) * | 1971-01-25 | 1972-11-21 | Witco Chemical Corp | Aqueous-based cosmetic detergent compositions |
-
1974
- 1974-07-25 FR FR7425834A patent/FR2283218A1/fr active Granted
-
1975
- 1975-01-01 AR AR259767A patent/AR206539A1/es active
- 1975-07-17 DE DE19752531925 patent/DE2531925A1/de not_active Withdrawn
- 1975-07-21 IL IL47748A patent/IL47748A/xx unknown
- 1975-07-22 AT AT564575A patent/AT343250B/de not_active IP Right Cessation
- 1975-07-22 NO NO752595A patent/NO752595L/no unknown
- 1975-07-23 DD DD187430A patent/DD122824A5/xx unknown
- 1975-07-24 LU LU73054A patent/LU73054A1/xx unknown
- 1975-07-24 AU AU83372/75A patent/AU8337275A/en not_active Expired
- 1975-07-24 ES ES439717A patent/ES439717A1/es not_active Expired
- 1975-07-24 IT IT25700/75A patent/IT1040009B/it active
- 1975-07-24 FI FI752136A patent/FI752136A7/fi not_active Application Discontinuation
- 1975-07-24 SE SE7508420A patent/SE7508420L/xx unknown
- 1975-07-25 OA OA55562A patent/OA05062A/xx unknown
- 1975-07-25 DK DK338675A patent/DK338675A/da unknown
- 1975-07-25 IE IE1676/75A patent/IE41641B1/en unknown
- 1975-07-25 CA CA232,293A patent/CA1079747A/en not_active Expired
- 1975-07-25 US US05/599,163 patent/US3996148A/en not_active Expired - Lifetime
- 1975-07-25 ZA ZA00754801A patent/ZA754801B/xx unknown
- 1975-07-25 JP JP50090334A patent/JPS5137103A/ja active Pending
- 1975-07-25 IN IN1463/CAL/75A patent/IN144017B/en unknown
- 1975-07-25 NL NL7508887A patent/NL7508887A/xx not_active Application Discontinuation
- 1975-07-25 CH CH978575A patent/CH597341A5/xx not_active IP Right Cessation
- 1975-07-25 GB GB31278/75A patent/GB1521984A/en not_active Expired
- 1975-07-25 BE BE158615A patent/BE831740A/xx unknown
- 1975-07-25 BR BR7504780*A patent/BR7504780A/pt unknown
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0008060A1 (de) * | 1978-08-03 | 1980-02-20 | BASF Aktiengesellschaft | Verwendung von mehrwertigen Alkoholen, (Hydroxy)carbonsäuren und/oder deren Estern mit den mehrwertigen Alkoholen als Viskositätsregler |
| EP0213475A3 (en) * | 1985-08-24 | 1988-01-13 | Bayer Ag | Polyesterpolyols, process for their fabrication and their utilisation in the isocyanate-polyaddition process |
Also Published As
| Publication number | Publication date |
|---|---|
| IE41641B1 (en) | 1980-02-13 |
| DK338675A (da) | 1976-01-26 |
| CH597341A5 (en, 2012) | 1978-03-31 |
| OA05062A (fr) | 1981-01-31 |
| FR2283218B1 (en, 2012) | 1977-03-18 |
| AU8337275A (en) | 1977-01-27 |
| IN144017B (en, 2012) | 1978-03-11 |
| LU73054A1 (en, 2012) | 1976-03-02 |
| CA1079747A (en) | 1980-06-17 |
| ZA754801B (en) | 1976-06-30 |
| BR7504780A (pt) | 1976-07-06 |
| AT343250B (de) | 1978-05-10 |
| AR206539A1 (es) | 1976-07-30 |
| DD122824A5 (en, 2012) | 1976-11-05 |
| NO752595L (en, 2012) | 1976-01-27 |
| IL47748A0 (en) | 1975-10-15 |
| FI752136A7 (en, 2012) | 1976-01-26 |
| IE41641L (en) | 1976-01-25 |
| FR2283218A1 (fr) | 1976-03-26 |
| JPS5137103A (en) | 1976-03-29 |
| ATA564575A (de) | 1977-09-15 |
| IT1040009B (it) | 1979-12-20 |
| SE7508420L (sv) | 1976-01-26 |
| NL7508887A (nl) | 1976-01-27 |
| US3996148A (en) | 1976-12-07 |
| ES439717A1 (es) | 1977-03-01 |
| BE831740A (fr) | 1975-11-17 |
| IL47748A (en) | 1979-03-12 |
| GB1521984A (en) | 1978-08-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 8139 | Disposal/non-payment of the annual fee |