JPS6362441B2 - - Google Patents
Info
- Publication number
- JPS6362441B2 JPS6362441B2 JP2008984A JP2008984A JPS6362441B2 JP S6362441 B2 JPS6362441 B2 JP S6362441B2 JP 2008984 A JP2008984 A JP 2008984A JP 2008984 A JP2008984 A JP 2008984A JP S6362441 B2 JPS6362441 B2 JP S6362441B2
- Authority
- JP
- Japan
- Prior art keywords
- acid
- quicklime
- granular
- calcium peroxide
- slaked lime
- 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.)
- Expired
Links
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 38
- 239000004343 Calcium peroxide Substances 0.000 claims description 21
- LHJQIRIGXXHNLA-UHFFFAOYSA-N calcium peroxide Chemical compound [Ca+2].[O-][O-] LHJQIRIGXXHNLA-UHFFFAOYSA-N 0.000 claims description 21
- 235000019402 calcium peroxide Nutrition 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000292 calcium oxide Substances 0.000 claims description 19
- 235000012255 calcium oxide Nutrition 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 12
- 239000000920 calcium hydroxide Substances 0.000 claims description 12
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 12
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 12
- 150000008043 acidic salts Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 159000000007 calcium salts Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 238000005502 peroxidation Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 235000019621 digestibility Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
産業上の利用分野
本発明は過酸化カルシウム組成物の新規な製造
方法に関する。
従来の技術
従来、過酸化カルシウムを得る方法としては、
消石灰スラリーまたは粉末に、過酸化水素水を反
応させて得るられる湿潤過酸化カルシウムを乾燥
する方法が知られている。しかし、この方法では
煩雑な乾燥工程が余分に必要である。
煩雑な乾燥工程を省くべく、反応後の湿潤過酸
化カルシウムに生石灰を投入してその水和熱で乾
燥する方法（特公昭58−30243号公報）が知られ
ている。
しかしながら、特公昭58−30243号公報の方法
は、一旦得られた湿潤過酸化カルシウムに、乾燥
と粉末化を目的として生石灰を投入するものであ
り、生成過酸化カルシウムの分解が起り、また、
遊離の消石灰が混入するという欠点があり、工程
的にも煩雑である。
また、以上のような従来法は何れも、元の生石
灰の多孔構造を残した機能性顆粒状ないし粉末状
の過酸化カルシウム組成物は製造できない。
本出願人は、先に生石灰を消化して消石灰を得
るに際し、生石灰と反応して水不溶性の塩を形成
する酸性基含有化合物（酸または塩）の水溶液を
添加することにより、品質の安定した、活性の高
い軽質粒状消石灰を製造することを提案した（特
公昭58−44611号公報）。この消石灰は、同公報に
も記載の通り、上記水溶液の添加量により見掛け
比重、硬度吸油量、活性度などの特性を変化させ
ることができ、使用目的に応じて特性を調整でき
ることから、機能性の高いものであつた。
発明が解決しようとする課題
本発明は、以上の点に鑑みて発明されたもので
あり、目的用途に応じた機能性顆粒状ないし粉末
状の過酸化カルシウム組成物を、乾燥工程を必要
とすることなく乾式で安価に得ることを目的とす
る。
発明の構成
即ち、本発明方法は、任意の粒度の生石灰に、
生石灰と反応して水に不溶性のカルシウム塩を生
成する酸または酸性塩の水溶液を反応せしめて、
顆粒状ないし粉状の消石灰を作り、次に過酸化水
素水を添加して過酸化反応と乾燥とを同時に進行
させることにより、顆粒状ないし粉状過酸化カル
シウム組成物を製造するものである。
本発明方法によれば、別途乾燥工程を必要とせ
ず、従来法の何れよりも簡単なプロセスで元の生
石灰の多孔構造を残した機能性顆粒状ないし粉末
状の過酸化カルシウム組成物を乾式で製造でき、
特公昭58−30243号公報のように一旦得られた過
酸化カルシウムに乾燥と粉末化を目的として生石
灰を投入することによる生成過酸化カルシウムの
分解とか、遊離の消石灰の混入という欠点もな
い。さらに、第一工程の処理で、マクロ構造、即
ち粒度（顆粒状、粉状）を調整でき、また、ミク
ロ構造（多孔質構造）も調整できる。
第１段階の顆粒状ないし粉状消石灰を得る工程
は、特公昭58−44611号公報に開示されている如
く、必要に応じ酸または酸性塩（以下、単に酸と
呼ぶこともある）の種類、濃度および添加量を決
めれば良く、そのメカニズムは酸の添加で消石灰
に自硬性を賦与するものである。酸または酸性塩
の種類としては、硫酸および硫酸塩が最も安価で
経済的である。その他の酸または酸性塩として
は、特公昭58−44611号に記載の通り、燐酸、珪
酸、珪弗化酸、ホウ酸、クロム酸、クエン酸、酒
石酸などであり、塩としてはAl、Zn、Mn、
NH3、Na、Ｋ等がある。
酸濃度および量と粒度とは正の相関を示し、酸
添加量が多いほど粗粒物（粒径0.245〜３mm）が
得られ、逆に酸添加量が少ないと粗粒物の収量が
低下して細粒物ないし粉状物（粒径0.245mm以下）
が多くなる。しかし、一方において、酸量が多く
なると例えば硫酸の場合は硫酸塩（石膏）が増加
して、有効CaO2量が減少するので、用途に応じ
て適宜選定される。本発明では次工程で過酸化と
同時に乾燥を行なう観点から、液量は生石灰重量
の40〜100重量％程度が良い。
次に、第２段階の顆粒状ないし粉状過酸化カル
シウム組成物を得る工程は、最終製品の過酸化カ
ルシウム含有量に見合つた過酸化水素水を添加す
ればよい。過酸化反応時の温度は、常法通り過酸
化水素の沸点以下に保つことが肝要で、過酸化水
素水の添加は反応温度に合せて投入すればよい。
具体的には、137℃で過酸化水素の蒸気圧が400mm
Hgに達し、かつ、分解するので、高価な過酸化
水素の歩留まりを考慮すると、135℃以下が好ま
しい。
このようにして得られる過酸化カルシウム組成
物は前述の如く、その目的に応じてミクロ（元の
生石灰の多孔構造を有する）およびマクロ（例え
ば、顆粒状、砂状、粉状）な形状並びに物性を賦
与することができる。例えば、農業用顆粒状品で
は生石灰の消化率を10〜40％に、過酸化率を50〜
85に制御し、24時間水中崩壊性を60％以上とす
る。また、水産用は、消化率20〜50％、過酸化率
50〜85％、水中崩壊率２％以下とし、白濁性およ
びPHの急上昇問題もなくすことができ、所望の仕
向先に適合した製品がモルタルミキサー等の簡単
な回転式反応機のみで任意に得られる。
発明の効果
本発明によれば、生石灰に、生石灰と反応して
水に不溶性のカルシウム塩を生成する酸または酸
性塩水溶液を反応せしめて消石灰を作り、次に過
酸化水素水を添加して過酸化反応と乾燥とを同時
に進行させることにより、乾式で顆粒状ないし粉
状の過酸化カルシウム組成物が得られる。
次に、本発明の特徴とするところを実施例によ
つて説明する。
実施例 １
３のステンレス製反応機に−10ｍ／ｍに破砕
した生石灰300ｇを採り、２容量％希硫酸溶液300
mlを加えて撹拌しながら反応させた。
反応終了後50℃以下になつた頃に、60％過酸化
水素水350mlを序々に加えながら撹拌し、乾燥し
た顆粒状の過酸化カルシウム組成物を得た。
このものの有効酸素量は17.8％であり、また、
その他の性状については後記表−１の通りであ
る。この過酸化カルシウム組成物は水分量18.6％
であるが、乾いた感じの十分に乾燥した組成物で
ある。
このものの有効酸素量は17.8％であつた。
過酸化水素水添加前後の顆粒状物のＸ線回折図
は第１図および第２図に示す通りであつた。過酸
化水素の添加により、Ca（OH）2ピークが小さく
なり、CaO2ピークが大きく現われることが判る。
なお、CaSO4のピークは第２図では明瞭に現われ
ていないが、試料調製（サンプリング）誤差の範
囲か、他ピークの影響かと考えられる。
実施例 ２
実施例１において、加える希硫酸溶液の濃度を
0.3％とした他は同様の方法で反応せしめ、乾い
た砂状ないし粉状の混合物より成る過酸化カルシ
ウム組成物を得た。
このものの有効酸素量は18.9％であり、その他
の性状は表−１に示した。
INDUSTRIAL APPLICATION FIELD OF THE INVENTION The present invention relates to a novel method for producing calcium peroxide compositions. Conventional technology Conventionally, the method for obtaining calcium peroxide is as follows:
A method of drying wet calcium peroxide obtained by reacting slaked lime slurry or powder with a hydrogen peroxide solution is known. However, this method requires an extra and complicated drying step. In order to eliminate the complicated drying process, a method is known in which quicklime is added to wet calcium peroxide after reaction and the calcium peroxide is dried using the heat of hydration (Japanese Patent Publication No. 30243/1983). However, in the method disclosed in Japanese Patent Publication No. 58-30243, quicklime is added to the wet calcium peroxide for the purpose of drying and pulverizing it, which causes decomposition of the produced calcium peroxide and
It has the disadvantage that free slaked lime is mixed in, and the process is complicated. Furthermore, none of the above conventional methods can produce functional granular or powdered calcium peroxide compositions that retain the original porous structure of quicklime. The present applicant has developed a method of stabilizing quality by adding an aqueous solution of an acidic group-containing compound (acid or salt) that reacts with quicklime to form a water-insoluble salt when first digesting quicklime to obtain slaked lime. proposed the production of highly active light granular slaked lime (Japanese Patent Publication No. 44611/1983). As stated in the same publication, the properties of this slaked lime, such as apparent specific gravity, hardness, oil absorption, and activity, can be changed depending on the amount of the aqueous solution added, and the properties can be adjusted depending on the purpose of use. It was a high price. Problems to be Solved by the Invention The present invention was invented in view of the above points, and it is possible to prepare a functional granular or powdered calcium peroxide composition according to the intended use, which requires a drying process. The purpose is to obtain it at a low cost by dry method without any process. Structure of the Invention That is, the method of the present invention is characterized in that quicklime of any particle size is
By reacting an acid or an aqueous solution of an acid salt that reacts with quicklime to form a water-insoluble calcium salt,
A granular or powdered calcium peroxide composition is produced by making granular or powdered slaked lime, then adding a hydrogen peroxide solution to allow the peroxidation reaction and drying to proceed simultaneously. According to the method of the present invention, a functional granular or powdered calcium peroxide composition that retains the original porous structure of quicklime can be produced in a dry process using a simpler process than any of the conventional methods without requiring a separate drying process. can be manufactured,
Unlike Japanese Patent Publication No. 58-30243, there are no disadvantages such as decomposition of the calcium peroxide produced by adding quicklime to the calcium peroxide once obtained for the purpose of drying and powdering, or contamination of free slaked lime. Furthermore, in the first step treatment, the macrostructure, that is, the particle size (granular, powdery) can be adjusted, and the microstructure (porous structure) can also be adjusted. As disclosed in Japanese Patent Publication No. 58-44611, the first stage step of obtaining granular or powdered slaked lime involves the use of the type of acid or acid salt (hereinafter sometimes simply referred to as acid), as required. The concentration and amount to be added can be determined, and the mechanism is to impart self-hardening properties to slaked lime by adding acid. Among the types of acids or acidic salts, sulfuric acid and sulfate are the cheapest and most economical. Other acids or acidic salts include phosphoric acid, silicic acid, silicofluoric acid, boric acid, chromic acid, citric acid, tartaric acid, etc. as described in Japanese Patent Publication No. 58-44611, and salts include Al, Zn, Mn,
Examples include NH 3 , Na, K, etc. There is a positive correlation between acid concentration and amount and particle size; the larger the amount of acid added, the more coarse particles (particle size 0.245 to 3 mm) will be obtained, and conversely, the smaller the amount of acid added, the lower the yield of coarse particles. fine particles or powder (particle size 0.245mm or less)
will increase. However, on the other hand, when the amount of acid increases, for example, in the case of sulfuric acid, the amount of sulfate (gypsum) increases and the effective amount of CaO 2 decreases, so it should be selected appropriately depending on the application. In the present invention, from the viewpoint of performing drying at the same time as peroxidation in the next step, the amount of liquid is preferably about 40 to 100% by weight of the quicklime. Next, in the second step of obtaining a granular or powdered calcium peroxide composition, a hydrogen peroxide solution suitable for the calcium peroxide content of the final product may be added. It is important to keep the temperature during the peroxidation reaction below the boiling point of hydrogen peroxide as usual, and the hydrogen peroxide solution may be added in accordance with the reaction temperature.
Specifically, the vapor pressure of hydrogen peroxide is 400mm at 137℃.
The temperature is preferably 135° C. or lower, considering the yield of expensive hydrogen peroxide, which reaches Hg and decomposes. As mentioned above, the calcium peroxide composition obtained in this way has micro (having the porous structure of the original quicklime) and macro (e.g. granular, sand-like, powder-like) shapes and physical properties depending on the purpose. can be granted. For example, for agricultural granules, the digestibility of quicklime is 10-40%, and the peroxidation rate is 50-40%.
85, with 24-hour disintegration in water of 60% or more. In addition, for marine products, the digestibility is 20 to 50%, and the peroxidation rate is 20% to 50%.
50 to 85%, disintegration rate in water is 2% or less, and the problem of white turbidity and rapid rise in pH can be eliminated, and products suitable for the desired destination can be obtained at any time using only a simple rotary reactor such as a mortar mixer. It will be done. Effects of the Invention According to the present invention, slaked lime is made by reacting quicklime with an acid or an aqueous acidic salt solution that reacts with quicklime to produce a water-insoluble calcium salt, and then hydrogen peroxide is added to make slaked lime. By allowing the oxidation reaction and drying to proceed simultaneously, a granular or powdery calcium peroxide composition can be obtained in a dry manner. Next, the features of the present invention will be explained using examples. Example 1 300 g of quicklime crushed to -10 m/m was placed in the stainless steel reactor of 3, and 300 g of 2% by volume dilute sulfuric acid solution was added.
ml was added and reacted with stirring. After the reaction was completed and the temperature reached 50° C. or below, 350 ml of 60% hydrogen peroxide solution was gradually added and stirred to obtain a dry granular calcium peroxide composition. The effective oxygen content of this product is 17.8%, and
Other properties are shown in Table 1 below. This calcium peroxide composition has a water content of 18.6%
However, it is a fairly dry composition with a dry feel. The effective oxygen content of this product was 17.8%. The X-ray diffraction patterns of the granules before and after addition of hydrogen peroxide solution were as shown in FIGS. 1 and 2. It can be seen that by adding hydrogen peroxide, the Ca(OH) 2 peak becomes smaller and the CaO 2 peak appears larger.
Note that although the CaSO 4 peak does not clearly appear in Figure 2, this is probably due to sample preparation (sampling) error or the influence of other peaks. Example 2 In Example 1, the concentration of the dilute sulfuric acid solution to be added was
The reaction was carried out in the same manner except that the amount was changed to 0.3% to obtain a calcium peroxide composition consisting of a dry sandy or powdery mixture. The effective oxygen content of this product was 18.9%, and other properties are shown in Table-1.
【表】【table】
第１図および第２図は過酸化水素添加前後の顆
粒状物のＸ線回折図である。
Figures 1 and 2 are X-ray diffraction patterns of the granules before and after addition of hydrogen peroxide.
Claims (1)
ルシウム塩を生成する酸または酸性塩水溶液を添
加して顆粒状ないし粉状の消石灰組成物を乾式で
得る工程と、次いで、これに過酸化水素水を加え
て過酸化物を乾式で得る工程とからなる、顆粒状
ないし粉状の過酸化カルシウム組成物の製造方
法。1. A step of dryly obtaining a granular or powdery slaked lime composition by adding to quicklime an acid or an aqueous acidic salt solution that reacts with the quicklime to produce a water-insoluble calcium salt, and then adding hydrogen peroxide to this. A method for producing a granular or powdery calcium peroxide composition, which comprises a step of dryly obtaining peroxide by adding water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008984A JPS60166204A (en) | 1984-02-08 | 1984-02-08 | Preparation of calcium peroxide composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008984A JPS60166204A (en) | 1984-02-08 | 1984-02-08 | Preparation of calcium peroxide composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60166204A JPS60166204A (en) | 1985-08-29 |
| JPS6362441B2 true JPS6362441B2 (en) | 1988-12-02 |
Family
ID=12017375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008984A Granted JPS60166204A (en) | 1984-02-08 | 1984-02-08 | Preparation of calcium peroxide composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60166204A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6265908A (en) * | 1985-09-12 | 1987-03-25 | Nippon Peroxide Co Ltd | Production of bivalent metal peroxide |
| GB9418984D0 (en) * | 1994-09-21 | 1994-11-09 | Solvay Interox Ltd | Low profile baffled reactor |
-
1984
- 1984-02-08 JP JP2008984A patent/JPS60166204A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60166204A (en) | 1985-08-29 |
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| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |