JPS63252926A - Production of fine particle powder of sodium trititanate - Google Patents
Production of fine particle powder of sodium trititanateInfo
- Publication number
- JPS63252926A JPS63252926A JP62086687A JP8668787A JPS63252926A JP S63252926 A JPS63252926 A JP S63252926A JP 62086687 A JP62086687 A JP 62086687A JP 8668787 A JP8668787 A JP 8668787A JP S63252926 A JPS63252926 A JP S63252926A
- Authority
- JP
- Japan
- Prior art keywords
- sodium
- raw material
- material compound
- titanium
- trititanate
- 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.)
- Granted
Links
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 31
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 31
- 239000011734 sodium Substances 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 title claims abstract description 13
- 239000010419 fine particle Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000002245 particle Substances 0.000 claims abstract description 26
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 239000011268 mixed slurry Substances 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000003463 adsorbent Substances 0.000 abstract description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 6
- 239000004408 titanium dioxide Substances 0.000 abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 5
- 235000017550 sodium carbonate Nutrition 0.000 abstract description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 abstract description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 abstract 1
- 238000010304 firing Methods 0.000 description 15
- 238000005342 ion exchange Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、イオン交換材あるいは吸着材として有用な三
チタン酸ナトリウム微細粒子粉末の製造法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing fine particle powder of sodium trititanate useful as an ion exchange material or adsorbent.
従来、三チタン酸ナトリウム微細粒子粉末の製造法とし
ては焼成法（吉用他、窯業協会誌、９４．７．１９８６
）が知られている。即ちこの製造方法は、二酸化チタン
と炭酸ナトリウムとを乾式混合して、８００℃で２Ｏ時
間焼成した後、粉砕、混合し、更に８００℃で２Ｏ時間
追焼成するという方法である。Conventionally, the firing method (Yoshiyuki et al., Journal of the Ceramics Industry Association, 94.7.1986
)It has been known. That is, this manufacturing method is a method in which titanium dioxide and sodium carbonate are dry mixed, fired at 800°C for 20 hours, pulverized, mixed, and further fired at 800°C for 20 hours.
本発明者らもこの製造方法により三チタン酸ナトリウム
微細粒子粉末の単−相の合成を試みたが、三チタン酸ナ
トリウムの単−相は得られたものの、粒子径は０１５〜
１０８ｍであって粒度分布範囲が広く、そのためイオン
交換材あるいは吸着材用として好ましいものではなかっ
た。即ち、三チタン酸ナトリウムは各種アルカリ金属イ
オンへの交換反応速度差を利用して水溶液中のリチウム
イオンを濃縮させるだめのイオン交換体の原料としての
検討が進められているが、このように反応速度差を利用
しである特定成分を濃縮させようとする場合、最高の分
離効率を示す反応時間が粒子径により異ることから、特
性を充分に発揮させるためにはイオン交換材あるいは吸
着材は狭い粒度分布を有する必要がある。The present inventors also attempted to synthesize a single phase of fine particle powder of sodium trititanate using this production method, but although a single phase of sodium trititanate was obtained, the particle size was
108 m, the particle size distribution range was wide, and therefore it was not preferable for use as an ion exchange material or an adsorbent. In other words, sodium trititanate is being considered as a raw material for an ion exchanger that can concentrate lithium ions in aqueous solutions by utilizing the difference in exchange reaction rates for various alkali metal ions. When attempting to concentrate a specific component by utilizing speed differences, the reaction time that shows the highest separation efficiency differs depending on the particle size, so in order to fully demonstrate its characteristics, it is necessary to use ion exchange materials or adsorbents. Must have a narrow particle size distribution.
また、前記従来法により単−相を得るためには、焼成、
粉砕、混合、焼成と、２度の焼成を必要とし、かつ各焼
成時間も２Ｏ時間という長時間を要するなど、工業的製
造法として利用が困難である。In addition, in order to obtain a single phase by the conventional method, calcination,
It is difficult to use as an industrial manufacturing method because it requires pulverization, mixing, and firing twice, and each firing time takes a long time of 20 hours.
このように従来の製造法は、イオン交換材あるいは吸着
材として有用な、狭い粒度分布を有する三チタン酸ナト
リウムを合成できないのみならず、製造法が煩雑であり
、経済的にも不利である等の欠点があった。As described above, conventional manufacturing methods not only cannot synthesize sodium trititanate with a narrow particle size distribution that is useful as an ion exchange material or adsorbent, but also are complicated and economically disadvantageous. There was a drawback.
そこで本発明はイオン交換材あるいは吸着材として有用
な、狭い粒度分布を有する三チタン酸ナトリウム微細粒
子粉末の経済的製造法を提供することを目的とする。SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide an economical method for producing finely divided sodium trititanate powder having a narrow particle size distribution and useful as an ion exchange material or adsorbent.
本発明者らは狭い粒度分布を有する三チタン酸ナトリウ
ム微細粒子粉末の経済的製造法を開発せんものと鋭意研
究の結果、ＴｉＯ２対Ｎａ２Ｏのモル比が３＝１の割合
で配合されているチタン原料化合物とナトリウム原料化
合物との混合スラリーを噴霧乾燥して、チタン原料化合
物の粒子表面にナトリウム原料化合物を均一に付着させ
た後、焼成することにより、狭い粒度分布を有する三チ
タン酸ナトリウム微細粒子からなる粒状物が得られ、次
いで該粒状物を水又は温水中に浸漬することにより、単
一粒子に分離した三チタン酸ナトリウム微細粒子粉末が
得られることを発見し、本発明を完成したものである。The present inventors have conducted extensive research to develop an economical manufacturing method for fine-particle powder of sodium trititanate with a narrow particle size distribution. A mixed slurry of the raw material compound and the sodium raw material compound is spray-dried to uniformly adhere the sodium raw material compound to the particle surface of the titanium raw material compound, and then fired to produce fine sodium trititanate particles with a narrow particle size distribution. The present invention was completed based on the discovery that fine particle powder of sodium trititanate separated into single particles could be obtained by immersing the granules in water or hot water. It is.
即ち、本発明の方法は、ＴｉＯ２対Ｎａ２Ｏのモル比が
３＝１の割合で配合されているチタン原料化合物とナト
リウム原料化合物との混合スラリーを噴霧乾燥した後、
７００〜１，１００℃で焼成して、三チタン酸ナトリウ
ム微細粒子からなる粒状物を生成せしめ、次いで該粒状
生成物を水又は温水中に浸漬して、微細単一粒子に分離
することを特徴とする。That is, in the method of the present invention, after spray-drying a mixed slurry of a titanium raw material compound and a sodium raw material compound in which the molar ratio of TiO2 to Na2O is 3=1,
It is characterized by firing at 700 to 1,100°C to produce a granular product consisting of fine particles of sodium trititanate, and then immersing the granular product in water or hot water to separate it into fine single particles. shall be.
本発明で使用されるチタン原料化合物としては二酸化チ
タン及び含水酸化チタンなどを挙げることができ、ナト
リウム原料化合物としては焼成時にＮａ２Ｏを生じる化
合物、例えばＮａ２Ｏ、Ｎ ａ ＯＨ％Ｎａ２ＣＯ３、
ＮａＨＣＯ３、Ｎａ２Ｃ２Ｏ４及びＮａＮＯ３などを挙
げることができる。Titanium raw material compounds used in the present invention include titanium dioxide and hydrous titanium oxide, and sodium raw material compounds include compounds that generate Na2O during firing, such as Na2O, NaOH%Na2CO3,
Mention may be made of NaHCO3, Na2C2O4 and NaNO3.
焼成温度は７００〜１，１００℃、好ましくは８００〜
ｉ、ｏｏｏ℃である。即ち焼成温度が１．Ｚｏ。Firing temperature is 700~1,100℃, preferably 800~
i,ooo°C. That is, the firing temperature is 1. Zo.
℃より高い場合には、三チタン酸ナトリウムの単−相を
得ることができず、一方焼成温度が７００℃よりも低い
と、反応速度が遅く、実用的でない。If the firing temperature is higher than 700°C, a single phase of sodium trititanate cannot be obtained. On the other hand, if the firing temperature is lower than 700°C, the reaction rate is slow and impractical.
尚、焼成時間は０．５〜１０時間、好ましくは１〜４時
間である。粒状生成物を単一の三チタン酸ナトリウム微
細粒子に分離する操作は、焼成物を適量の水又は温水中
に投入して、０．５〜ｌＯ時間浸漬後、攪拌することに
よりなされる。Incidentally, the firing time is 0.5 to 10 hours, preferably 1 to 4 hours. The operation of separating the granular product into single fine particles of sodium trititanate is carried out by putting the calcined product into an appropriate amount of water or warm water, immersing it for 0.5 to 10 hours, and then stirring.
以下、実施例及び比較例たより、本発明を更に詳しく説
明する。The present invention will be explained in more detail below with reference to Examples and Comparative Examples.
実施例１゜
アナターゼ型二酸化チタン１，０００ｇ及び炭酸ナトリ
ウム４４２ｇを秤量し、２．５Ｌの水を添加稜、よく攪
拌した。このスラリーを入口温度２７０〜２８０℃、出
口温度８０〜８５℃の条件で噴霧乾燥した。Example 1 1,000 g of anatase-type titanium dioxide and 442 g of sodium carbonate were weighed, 2.5 L of water was added, and the mixture was thoroughly stirred. This slurry was spray-dried under conditions of an inlet temperature of 270 to 280°C and an outlet temperature of 80 to 85°C.
次に、この乾燥物をアルミナ製ルツボに入れ、電気炉中
で昇温速度２Ｏ０℃／時、焼成温度８５０℃、保持時間
４時間の条件で焼成した後、２Ｏ０℃／時の速度で降温
した。Next, this dried product was placed in an alumina crucible and fired in an electric furnace at a heating rate of 200°C/hour, a firing temperature of 850°C, and a holding time of 4 hours, and then the temperature was lowered at a rate of 200°C/hour. .
焼成物をステンレス製容器中のＩＯＬの温水に投入して
、３時間浸漬した後ホモミキサーで１時間攪拌し、次い
でろ過、洗浄、乾燥して、チタン酸ナトリウム微細粉末
を得た。The calcined product was put into the warm water of an IOL in a stainless steel container, immersed for 3 hours, stirred for 1 hour using a homomixer, and then filtered, washed, and dried to obtain a fine powder of sodium titanate.
この生成物をＸ線回折により同定したところ、三チタン
酸ナトリウムの単−相であった。又走査型電子顕微鏡に
より観察したところ、粒子径０．４〜０．７μｍ１粒子
長２〜４μｍの柱状結晶であったＯ
実施例２゜
Ｔｉ０２３１．４％、５Ｏａ２．３％を含む含水酸化チ
タンスラリー２，６００Ｆを攪拌しながら、炭酸ナトリ
ウム粉末４４０ｇを添加した。このスラリーを実施例１
．と同様な条件で噴霧乾燥した。This product was identified by X-ray diffraction and was found to be a single phase of sodium trititanate. Further, when observed with a scanning electron microscope, O was found to be columnar crystals with a particle diameter of 0.4 to 0.7 μm and a particle length of 2 to 4 μm. While stirring at 2,600F, 440g of sodium carbonate powder was added. This slurry was used in Example 1.
．． Spray-dried under the same conditions.
次にこの乾燥物をアルミナ製ルツボに入れ、電気炉で昇
温速度２Ｏ０℃／時、焼成温度１，０００℃、保持時間
２時間の条件で焼成した後、２Ｏ０℃／時の速度で降温
した。Next, this dried product was placed in an alumina crucible and fired in an electric furnace at a heating rate of 200°C/hour, a firing temperature of 1,000°C, and a holding time of 2 hours, and then the temperature was lowered at a rate of 200°C/hour. .
焼成物をステンレス製容器中の８Ｌの温水に投入して、
５時間浸漬した後、ホモミキサーで１時間攪拌し、次い
でろ過、洗浄、乾燥して、チタン酸ナトリウム微細粉末
を得た。Pour the baked product into 8L of warm water in a stainless steel container,
After being immersed for 5 hours, the mixture was stirred for 1 hour using a homomixer, and then filtered, washed, and dried to obtain a fine powder of sodium titanate.
この生成物をＸ線回折により同定したところ、三チタン
酸ナトリウムの単−相であった。又走査型電子顕微鏡に
より観察したところ、粒子径０．８〜１．３μｍ１ 粒
子長３〜５μｍの柱状結晶であった０
比較例１゜
アナターゼ型二酸化チタン１００ｇと炭酸ナトリウム４
４．２ｐを秤量し、石川式播漬機で湿式混合した後、ア
ルミナ製ルツボに入れ、電気炉中で昇温速度２Ｏ０℃／
時、焼成温度８００℃、保持時間２Ｏ時間の条件で焼成
した後、２Ｏ０℃／時の速度で降温した。This product was identified by X-ray diffraction and was found to be a single phase of sodium trititanate. When observed using a scanning electron microscope, the particles were columnar crystals with a particle diameter of 0.8 to 1.3 μm and a particle length of 3 to 5 μm.Comparative Example 1: 100 g of anatase-type titanium dioxide and 4
After weighing 4.2p and wet mixing with an Ishikawa-type sowing machine, it was placed in an alumina crucible and heated at a heating rate of 2O0℃/in an electric furnace.
After firing at a firing temperature of 800° C. and a holding time of 20 hours, the temperature was lowered at a rate of 200° C./hour.
焼成物をＸ線回折により同定したところ、三チタン酸ナ
トリウム、六チタン酸ナトリウム及び二酸化チタンから
なる混合相であった０
次に、この焼成物を石川式拙漬機で粉砕、混合した後、
１回目と同様な条件で追焼成した。これにより得られた
生成物はＸ線回折により三チタン酸ナトリウムの単−相
であることが判った。又走査型電子顕微鏡により観察し
たところ、０．５〜２μｍの大きさの粒状粒子と粒子径
１〜２μｍ、長さ５〜１０μｍの柱状粒子との混合物で
あり、実施例１．及び２．で得られた生成物よりも明ら
かに粒度分布の悪いものであった。When the fired product was identified by X-ray diffraction, it was found to be a mixed phase consisting of sodium trititanate, sodium hexatitanate, and titanium dioxide.Next, this fired product was crushed and mixed in an Ishikawa-style pickling machine, and then
Additional firing was performed under the same conditions as the first time. The product thus obtained was found to be a single phase of sodium trititanate by X-ray diffraction. Further, when observed using a scanning electron microscope, it was found that it was a mixture of granular particles with a size of 0.5 to 2 μm and columnar particles with a particle diameter of 1 to 2 μm and a length of 5 to 10 μm. and 2. The particle size distribution was clearly worse than that of the product obtained in .
発明の効果
本発明による製造法は従来法よりも経済的に有利のみな
らず、本発明の製造法により得られる三チタン酸ナトリ
ウム微細粉末は、従来法により得られる三チタン酸ナト
リウム微細粉末よりも狭い粒度分布を有する為、イオン
交換材及び吸着材用として好適である。Effects of the Invention The production method according to the present invention is not only more economically advantageous than the conventional method, but also the sodium trititanate fine powder obtained by the production method of the present invention is superior to the sodium trititanate fine powder obtained by the conventional method. Since it has a narrow particle size distribution, it is suitable for use as ion exchange materials and adsorbents.
特許出願人 チタン工業株式会社 （外５名）Patent applicant: Titanium Industries Co., Ltd. (5 other people)
Claims (1)
されているチタン原料化合物とナトリウム原料化合物と
の混合スラリーを噴霧乾燥した後、７００〜１，１００
℃で焼成して、三チタン酸ナトリウム微細粒子からなる
粒状物を生成せしめ、次いで該粒状生成物を水又は温水
中に浸漬して、単一粒子に分離することを特徴とする、
三チタン酸ナトリウム微細粒子粉末の製造法。After spray-drying a mixed slurry of a titanium raw material compound and a sodium raw material compound in which the molar ratio of TiO_2 to Na_2O is 3:1, 700 to 1,100
C. to produce a granular product consisting of fine particles of sodium trititanate, and then immersing the granular product in water or hot water to separate it into single particles.
A method for producing fine particle powder of sodium trititanate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086687A JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086687A JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63252926A true JPS63252926A (en) | 1988-10-20 |
| JPH0832557B2 JPH0832557B2 (en) | 1996-03-29 |
Family
ID=13893900
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62086687A Expired - Fee Related JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0832557B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7013067B1 (en) * | 2020-11-02 | 2022-01-31 | 国立大学法人信州大学 | Filtration material, manufacturing method of filtration material, water treatment material and water purifier |
| WO2022091514A1 (en) * | 2020-11-02 | 2022-05-05 | 国立大学法人信州大学 | Filter material, production method for filter material, water treatment material, and water purifier |
-
1987
- 1987-04-08 JP JP62086687A patent/JPH0832557B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7013067B1 (en) * | 2020-11-02 | 2022-01-31 | 国立大学法人信州大学 | Filtration material, manufacturing method of filtration material, water treatment material and water purifier |
| WO2022091514A1 (en) * | 2020-11-02 | 2022-05-05 | 国立大学法人信州大学 | Filter material, production method for filter material, water treatment material, and water purifier |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0832557B2 (en) | 1996-03-29 |
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| R250 | Receipt of annual fees |
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| LAPS | Cancellation because of no payment of annual fees |