JPH03137008A - Production of tellurium dioxide - Google Patents
Production of tellurium dioxideInfo
- Publication number
- JPH03137008A JPH03137008A JP27381089A JP27381089A JPH03137008A JP H03137008 A JPH03137008 A JP H03137008A JP 27381089 A JP27381089 A JP 27381089A JP 27381089 A JP27381089 A JP 27381089A JP H03137008 A JPH03137008 A JP H03137008A
- Authority
- JP
- Japan
- Prior art keywords
- tellurium
- solution
- metal
- dioxide
- tecl4
- 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.)
- Pending
Links
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- 229910052714 tellurium Inorganic materials 0.000 claims description 31
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 31
- OFDISMSWWNOGFW-UHFFFAOYSA-N 1-(4-ethoxy-3-fluorophenyl)ethanamine Chemical compound CCOC1=CC=C(C(C)N)C=C1F OFDISMSWWNOGFW-UHFFFAOYSA-N 0.000 claims description 25
- 239000002245 particle Substances 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000010908 decantation Methods 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- SWLJJEFSPJCUBD-UHFFFAOYSA-N tellurium tetrachloride Chemical compound Cl[Te](Cl)(Cl)Cl SWLJJEFSPJCUBD-UHFFFAOYSA-N 0.000 abstract 5
- 229910003069 TeO2 Inorganic materials 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 16
- 238000006460 hydrolysis reaction Methods 0.000 description 12
- 230000007062 hydrolysis Effects 0.000 description 11
- 239000002253 acid Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000005297 pyrex Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は光学用単結晶等の素材として使用される二酸化
テルルの製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing tellurium dioxide, which is used as a material for optical single crystals and the like.
［従来の技術］
二酸化テルルは一般に化学薬品として使用されるが、純
度９９．９９９重量％（以下％と示す。）以上の二酸化
テルルを原料として単結晶とした物は、レーザープリン
ター、カラースキャナー、スペクトラムアナライザー等
の超音波光変調器、偏光器等の特殊用途に最適とされて
いる。このような光学的単結晶製造用二酸化テルルとし
ては、純度のみならず、吸着ガス量の少ない正方晶系の
粗大結晶が望まれている。[Prior Art] Tellurium dioxide is generally used as a chemical, but single crystals made from tellurium dioxide with a purity of 99.999% by weight or higher (hereinafter referred to as %) can be produced using laser printers, color scanners, It is ideal for special applications such as ultrasonic optical modulators such as spectrum analyzers and polarizers. As tellurium dioxide for producing optical single crystals, it is desired to have not only high purity but also coarse tetragonal crystals with a small amount of adsorbed gas.
従来、二酸化テルルは金属テルルと濃硝酸とを反応させ
て塩基性硝酸塩を？幸、これを加熱分解する方法で製造
されている。しかし、この方法では、反応時に金属テル
ルの表面に酸化テルルが生成し、金属テルルの溶解を停
止させてしまい、金属テルルを充分に溶解できないとい
う欠点を持っている。Traditionally, tellurium dioxide was produced by reacting metallic tellurium with concentrated nitric acid to form basic nitrate. Fortunately, it is manufactured by thermally decomposing it. However, this method has the disadvantage that tellurium oxide is generated on the surface of the tellurium metal during the reaction, stopping the dissolution of the tellurium metal, and the tellurium metal cannot be sufficiently dissolved.
更に、この方法で得られる結晶は必ずしも正方晶系の物
ではなく、２０μｍ以下の黄色味を帯びた斜方晶系の結
晶となることが多い。Further, the crystals obtained by this method are not necessarily tetragonal, but are often yellowish orthorhombic crystals with a diameter of 20 μm or less.
この欠点を解消すべく金属テルルに乾燥塩素ガスを作用
させ、四塩化テルルを生ぜしめ、これを蒸留精製した後
に純水により加水分解して二酸化テルルを得る方法が特
開昭６３−２８６５３１号に開示されている。In order to overcome this drawback, a method was proposed in JP-A-63-286531 in which tellurium metal is treated with dry chlorine gas to produce tellurium tetrachloride, which is purified by distillation and then hydrolyzed with pure water to obtain tellurium dioxide. Disclosed.
［発明が解決しようとする課題］
しかし、上記方法は、確かに金属テルルを充分に溶解で
き、高純度の二酸化テルルが得られるものの、腐食性の
強い塩素ガスを４００’Ｃ以上の高温度で金属テルルと
反応させるため、石英製の装置を使用せざるを得ず、高
コストにならざるを得ないばかりか、環境上も好ましく
ないという問題がある。[Problems to be Solved by the Invention] However, although the above method can certainly dissolve metallic tellurium sufficiently and produce high-purity tellurium dioxide, it does not require the use of highly corrosive chlorine gas at a high temperature of 400'C or higher. In order to react with metallic tellurium, a device made of quartz must be used, which is not only expensive but also environmentally unfavorable.
本発明の目的は、上記問題点のない正方品系の３０μｍ
以上の二酸化テルル結晶の製造方法の提供にある。The object of the present invention is to produce a 30 μm square product without the above-mentioned problems.
The present invention provides a method for producing the above tellurium dioxide crystal.
［課題を解決するための手段］
上記課題を解決する本発明の方法は、金属テルルを、金
属テルルに対して１〜２当量、好ましくは１．２〜１．
５当量の塩酸と、該塩酸に対して容量比で２０〜４０％
の硝酸と加えて溶解し、固液分離して四塩化テルル溶液
を得、該四塩化テルル溶液を、該溶液に対して重量で１
０倍以上、好ましくは１０〜２０倍の７０〜９５℃１好
ましくは８０〜９０℃の温水に、液温を７０〜９５℃１
好ましくは８０〜９０℃に維持しつつ添加し、四塩化テ
ルルを加水分解して二酸化テルルを得るものである。[Means for Solving the Problems] The method of the present invention for solving the above problems includes using tellurium metal in an amount of 1 to 2 equivalents, preferably 1.2 to 1.0 equivalents, relative to tellurium metal.
5 equivalents of hydrochloric acid and 20 to 40% by volume relative to the hydrochloric acid
of nitric acid and dissolve, solid-liquid separation is performed to obtain a tellurium tetrachloride solution, and the tellurium tetrachloride solution is added to
0 times or more, preferably 10 to 20 times as much hot water at 70 to 95 degrees Celsius, preferably 80 to 90 degrees Celsius, and the liquid temperature to 70 to 95 degrees Celsius.
Preferably, it is added while maintaining the temperature at 80 to 90°C, and tellurium tetrachloride is hydrolyzed to obtain tellurium dioxide.
［作用］
本発明で用いる塩酸及び硝酸は、それぞれ濃塩酸、濃硝
酸である。これは、各酸の濃度が低いと生成した四塩化
テルルが加水分解して二酸化テルルを生成し、沈殿する
ためである。一般に知られているように金属テルルは塩
酸にほとんど溶解しないが、この混合溶液に硝酸を加え
ると金属テルルが溶解し始める。加える硝酸の量が少な
いと溶解する金属テルルの溶解が不十分となるので、加
える硝酸の量は塩酸に対して容量比で２０％以上とする
ことが必要である。しかし、加える硝酸の量を多くして
も、反応により生成するＮＯｘの量が増加するのみであ
り、溶解自体にはさほど影響を与えない。よって、加え
る硝酸の量は塩酸に対して容量比で４０％以下とするこ
とが望ましい。[Function] Hydrochloric acid and nitric acid used in the present invention are concentrated hydrochloric acid and concentrated nitric acid, respectively. This is because when the concentration of each acid is low, the produced tellurium tetrachloride is hydrolyzed to produce tellurium dioxide, which is precipitated. As is generally known, metallic tellurium hardly dissolves in hydrochloric acid, but when nitric acid is added to this mixed solution, metallic tellurium begins to dissolve. If the amount of nitric acid added is small, the metal tellurium will be insufficiently dissolved, so the amount of nitric acid added needs to be 20% or more by volume relative to hydrochloric acid. However, even if the amount of nitric acid added is increased, the amount of NOx generated by the reaction will only increase, and the dissolution itself will not be affected much. Therefore, it is desirable that the amount of nitric acid added be 40% or less by volume relative to hydrochloric acid.
なお、金属テルルの溶解方法としてこのように塩酸中に
金属テルルを投入し、これに硝酸を加えても良く、また
予め混酸を作成しておき、これと金属テルルとを反応さ
せても良い。Note that as a method for dissolving metal tellurium, metal tellurium may be poured into hydrochloric acid as described above and nitric acid may be added thereto, or a mixed acid may be prepared in advance and this and metal tellurium may be reacted.
上記のように金属テルルを溶解するが、この際に加える
塩酸の量が金属テルルの当量を越えると、金属テルルの
ほとんどが溶解して微細な灰色の固形物が生じる。加え
る塩酸の量が金属テルルの２．５当量以上になるとこの
固形物は完全に溶解してしまう。この灰色の固形物が何
かということについては不明であるが、得られる最終製
品である二酸化テルルの色、結晶系等の諸性質に対して
この灰色の固形分を溶解することは好ましくない。Metal tellurium is dissolved as described above, but if the amount of hydrochloric acid added at this time exceeds the equivalent amount of metal tellurium, most of the metal tellurium is dissolved and a fine gray solid is produced. If the amount of hydrochloric acid added exceeds 2.5 equivalents of metal tellurium, this solid will completely dissolve. Although it is unclear what this gray solid is, it is undesirable to dissolve this gray solid in view of the color, crystal system, and other properties of the final product obtained, tellurium dioxide.
そのため、金属テルルと反応させる塩酸量は金属テルル
に対して２当量以下とすることが必要であり、好ましく
は１．５当ｍ以下とすることが望ましい。よって、この
ようにして得られた溶解液には灰色の固形物が浮遊して
いることとなり、四塩化テルルの加水分解により高純度
の二酸化テルルを得るためには、この固形物を固液分離
して除去しなければならない。なお、固液分離法として
採用すべき手段は特に限定されるものではない。Therefore, the amount of hydrochloric acid to be reacted with metal tellurium needs to be 2 equivalents or less, preferably 1.5 equivalents or less relative to metal tellurium. Therefore, gray solid matter is suspended in the solution obtained in this way, and in order to obtain high-purity tellurium dioxide by hydrolyzing tellurium tetrachloride, this solid matter must be separated into solid-liquid. must be removed. Note that the means to be adopted as the solid-liquid separation method is not particularly limited.
得られた四塩化テルル溶液より二酸化テルルを得るには
四塩化テルル溶液を大量の水に添加し、加水分解反応を
起こさせるがこの際の四塩化テルル溶液の添加速度や加
水分解温度や使用する水の量が生成する二酸化テルルの
粒径に大きく影響する。To obtain tellurium dioxide from the resulting tellurium tetrachloride solution, the tellurium tetrachloride solution is added to a large amount of water to cause a hydrolysis reaction, but the rate of addition of the tellurium tetrachloride solution, the hydrolysis temperature, and the use The amount of water greatly affects the particle size of the tellurium dioxide produced.
一般に添加速度を遅くすると、最初に生成された種晶に
二酸化テルルが析出し、結晶を粗大化させるが、本発明
の場合には、加水分解温度を一定に維持しつつ四塩化テ
ルルを添加するために添加速度は遅くせざるを得す、そ
の結果、添加速度の粒径に与える効果は相対的に微小と
なり、加水分解温度や使用する水の量の効果が大きくな
ると思われる。例えば、常温では、溶解に用いた混酸の
量や水の量のいかんにかかわらず、２〜３μｍ程度の結
晶しか生成せず、加水分解温度を６０℃とし、溶解時の
混酸の量を、該混酸中の塩酸量が金属テルルの１．２当
量となるようにして得た四塩化テルル溶液と、該四塩化
テルル溶液に対して重量で１５倍程度の純水とを用いて
加水分解を行なうと５〜１５μｍの粒径の二酸化テルル
が得られ、加水分解温度を９０℃とし、溶解時の混酸の
量を、該混酸中の塩酸量が金属テルルの１．２当量とな
るようにしてえた四塩化テルル溶液と、該四塩化テルル
溶液に対して重量で１０倍程度の純水とを用いて加水分
解を行なうと２０〜２５μｍの粒径の二酸化テルルが得
られる。このように、溶解時に使用した酸の量と加水分
解時の温度が得られる二酸化テルルの粒径に影響を与え
るのは、加水分解中の液への二酸化テルルの溶解度が、
二酸化テルルを溶解し、再結晶する工程を繰返して結晶
の成長が起きる程度にあるからであると思われる。Generally, when the addition rate is slowed, tellurium dioxide precipitates in the initially generated seed crystals, causing the crystals to become coarse, but in the case of the present invention, tellurium tetrachloride is added while maintaining the hydrolysis temperature constant. Therefore, the addition rate has to be slow, and as a result, the effect of the addition rate on the particle size is thought to be relatively small, while the effect of the hydrolysis temperature and the amount of water used becomes large. For example, at room temperature, regardless of the amount of mixed acid or water used for dissolution, only crystals of about 2 to 3 μm are formed. Hydrolysis is carried out using a tellurium tetrachloride solution obtained such that the amount of hydrochloric acid in the mixed acid is 1.2 equivalents of metal tellurium, and pure water about 15 times the weight of the tellurium tetrachloride solution. Tellurium dioxide with a particle size of 5 to 15 μm was obtained, the hydrolysis temperature was set to 90°C, and the amount of mixed acid during dissolution was such that the amount of hydrochloric acid in the mixed acid was 1.2 equivalents of metal tellurium. When hydrolysis is carried out using a tellurium tetrachloride solution and pure water about 10 times the weight of the tellurium tetrachloride solution, tellurium dioxide having a particle size of 20 to 25 μm is obtained. Thus, the amount of acid used during dissolution and the temperature during hydrolysis affect the particle size of the resulting tellurium dioxide.The solubility of tellurium dioxide in the liquid during hydrolysis is
This is thought to be due to the fact that the process of dissolving and recrystallizing tellurium dioxide is repeated to the extent that crystal growth occurs.
ところで、使用する水の量が少ないと二酸化テルルの溶
解度が上昇し、四塩化テルルは充分に分解せず、また得
られる結晶中のＣＩ−やＮＯ”−含量が高（なる。一方
、また、あまりに水が多いと取扱に不便である。By the way, if the amount of water used is small, the solubility of tellurium dioxide increases, tellurium tetrachloride is not decomposed sufficiently, and the CI- and NO"- contents in the obtained crystals are high. On the other hand, Too much water is inconvenient to handle.
本発明の目的である３０〜５０μｍの粒径の二酸化テル
ルを得るためには、溶解時に使用する混酸の量を、該混
酸中の塩酸量が金属テルルに対して１．２当量以上とす
ることが必要であり、加水分解時の温度を７５〜９５℃
１好ましくは８゜〜９０℃とし、用いる水の量を１０倍
以上とすることが必要であり、好ましくは１０〜２０倍
とすることが望ましい。In order to obtain tellurium dioxide with a particle size of 30 to 50 μm, which is the objective of the present invention, the amount of mixed acid used during dissolution should be such that the amount of hydrochloric acid in the mixed acid is 1.2 equivalents or more relative to metal tellurium. is required, and the temperature during hydrolysis is 75-95℃.
1. The temperature is preferably 8° to 90°C, and the amount of water used must be 10 times or more, preferably 10 to 20 times.
なお、用いる水は得られる二酸化テルルの純度を高める
ためには純水が望ましい。In addition, the water used is preferably pure water in order to increase the purity of the obtained tellurium dioxide.
［実施例−１］
純度９９．９９％の塊状金属テルル１．ＯＫｇを容１１
０ Ｖχのパイレックス製ビーカーに入れた後、濃塩酸
４．２ｉ’Ｚ、及び濃硝酸１．４′ＩＺを添加し、２０
時間放置した。得られた溶液中の未溶解物をグラスフィ
ルターを用いてろ過し、四塩化テルル溶液を得た。次い
で、テフロンライニングを施した加水分解漕に純水１５
０７Ｚを入れ、チタン裂損はん羽根を備えた攪はん機で
攪はんしつつ、９０’Ｃまで昇温し、前記四塩化テルル
溶液７．８ Ｋｇを３０分間かけて添加し、沈殿を得、
これをデカンテーションにより分離後、１５Ｑ ｉ’λ
の純水を用いて、室温で２回洗浄し、６０℃で１回洗浄
し、乾燥して１．１Ｋｇの二酸化テルルを得た。この二
酸化テルルを分析したところ、Ｆｅ Ｏ，Ｌ Ｎｉ
Ｏ，１、Ｃｕく１、 Ｓｅ ＜０．５、 ＣＩ−
＜１００、 ＮＯ３−＜１００ 各 ｐｐｍであり、
また、ＢＥＴ比表面積計で測定した平均粒径は３６μｍ
であり、Ｘ線回折で測定した結果、正方晶のみであるこ
とがわかった。[Example-1] Bulk metallic tellurium with a purity of 99.99% 1. OKg capacity 11
After placing in a Pyrex beaker with 0 Vχ, 4.2 i'Z of concentrated hydrochloric acid and 1.4'IZ of concentrated nitric acid were added, and 20
I left it for a while. Undissolved substances in the obtained solution were filtered using a glass filter to obtain a tellurium tetrachloride solution. Next, 15 liters of pure water was added to a Teflon-lined hydrolysis tank.
07Z was added, the temperature was raised to 90'C while stirring with a stirrer equipped with a titanium breakage blade, and 7.8 kg of the tellurium tetrachloride solution was added over 30 minutes to precipitate. obtained,
After separating this by decantation, 15Q i'λ
The product was washed twice at room temperature with pure water, once at 60° C., and dried to obtain 1.1 kg of tellurium dioxide. Analysis of this tellurium dioxide revealed that FeO, LNi
O,1, Cu1, Se <0.5, CI-
<100, NO3-<100 each ppm,
In addition, the average particle size measured with a BET specific surface area meter was 36 μm.
As a result of measurement by X-ray diffraction, it was found that it was only a tetragonal crystal.
［実施例−２コ
純度９９．９９％の塊状金属テルル２．ＯＫｇを容！
２０ ？Ｚのパイレックス製ビーカーに入れた後、濃塩
酸８．４ｖχ、及び濃硝酸２．８ｖＺを添加し、２０時
間放置した。得られた溶液中の未溶解物をグラスフィル
ターを用いてろ過し、四塩化テルル溶液を得た。次いで
、テフロンライニングを施した加水分解漕に純水ｌ５Ｃ
ＩＺを入れ、チタン裂損はん羽根を備えた攪はん機で攪
はんしつつ、９０℃まで昇温し、前記四塩化テルル溶液
１５．５ Ｋｇを３０分間かけて添加し、沈殿を得、こ
れをデカンテーションにより分離後、１５０″ｌλの純
水を用いて、室温で２回洗浄し、６０℃で１回洗浄し、
乾燥しテ２．０ Ｋｇの二酸化テルルを得た。この二酸
化テルルを分析したところ、Ｆｅ Ｏ，ｆ、Ｎｉ
Ｃ１，Ｌ Ｃｕく１、 Ｓｅ ＜０．５、ＣＩ−＜
１００、ＮＯ３−＜１００ 各 ｐｐｍであり、また
、ＢＥＴ比表面積計で測定した平均粒径は５３μｍであ
り、Ｘ線回折で測定した結果、正方晶のみであることが
わかった。[Example 2] Bulk metallic tellurium with a purity of 99.99% 2. OKg!
20? After placing the mixture in a Pyrex beaker Z, 8.4 vx of concentrated hydrochloric acid and 2.8 v of concentrated nitric acid were added, and the mixture was left to stand for 20 hours. Undissolved substances in the obtained solution were filtered using a glass filter to obtain a tellurium tetrachloride solution. Next, pure water 15C was added to a Teflon-lined hydrolysis tank.
IZ was added, the temperature was raised to 90°C while stirring with a stirrer equipped with a titanium breakage blade, and 15.5 kg of the tellurium tetrachloride solution was added over 30 minutes to remove the precipitate. After separating this by decantation, it was washed twice at room temperature and once at 60°C using 150″lλ of pure water,
After drying, 2.0 kg of tellurium dioxide was obtained. When this tellurium dioxide was analyzed, it was found that FeO, f, Ni
C1,L Cu1, Se <0.5, CI-<
100, NO3-<100 ppm each, and the average particle diameter measured by a BET specific surface area meter was 53 μm, and the result of measurement by X-ray diffraction revealed that it was only a tetragonal crystal.
［発明の効果］
本発明の方法によれば、容易に粒径３０μｍ以上の正方
晶系の粗大結晶を得ることができるばかりでなく、得ら
れる粒子は着色せず、光学的単結晶製造用二酸化テルル
として最適である。[Effects of the Invention] According to the method of the present invention, not only can tetragonal coarse crystals with a particle size of 30 μm or more be easily obtained, but the resulting particles are not colored and are suitable for use in producing optical single crystals. It is most suitable as tellurium.
更に、本発明の方法を利用すれば、得られる二酸化テル
ルの粒径を任意に調節することも可能である。Furthermore, by using the method of the present invention, it is also possible to arbitrarily adjust the particle size of the tellurium dioxide obtained.
Claims (2)
塩酸と、該塩酸に対して容量比で２０％以上の硝酸とを
加えて溶解し、固液分離して四塩化テルル溶液を得、該
四塩化テルル溶液を、該溶液に対して重量で１０倍以上
の７０〜９５℃の温水に、液温を７０〜９５℃に維持し
つつ添加し、四塩化テルルを加水分解して二酸化テルル
を得ることを特徴とする二酸化テルルの製造方法。(1) Metal tellurium is dissolved by adding 1 to 2 equivalents of hydrochloric acid to the metal tellurium and nitric acid with a volume ratio of 20% or more to the hydrochloric acid, followed by solid-liquid separation to obtain a tellurium tetrachloride solution. The tellurium tetrachloride solution obtained is added to 70 to 95 °C hot water at least 10 times the weight of the solution while maintaining the liquid temperature at 70 to 95 °C, and the tellurium tetrachloride is hydrolyzed. A method for producing tellurium dioxide, characterized by obtaining tellurium dioxide.
５当量の濃塩酸と、該濃塩酸に対して容量比で２０〜４
０％の濃硝酸とを加えて溶解し、固液分離して四塩化テ
ルル溶液を得、該四塩化テルル溶液を、該溶液に対して
重量で１０〜２０倍の８０〜９０℃の温水に、液温を８
０〜９０℃に維持しつつ添加し、四塩化テルルを一加水
分解して二酸化テルルを得ることを特徴とする二酸化テ
ルルの製造方法。(2) Metal tellurium is 1.2 to 1.
5 equivalents of concentrated hydrochloric acid and a volume ratio of 20 to 4 equivalents to the concentrated hydrochloric acid.
Add 0% concentrated nitric acid to dissolve, solid-liquid separation to obtain a tellurium tetrachloride solution, and add the tellurium tetrachloride solution to 80 to 90°C warm water of 10 to 20 times the weight of the solution. , liquid temperature 8
A method for producing tellurium dioxide, which comprises adding tellurium tetrachloride while maintaining the temperature at 0 to 90°C and monohydrolyzing tellurium dioxide to obtain tellurium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27381089A JPH03137008A (en) | 1989-10-23 | 1989-10-23 | Production of tellurium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27381089A JPH03137008A (en) | 1989-10-23 | 1989-10-23 | Production of tellurium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03137008A true JPH03137008A (en) | 1991-06-11 |
Family
ID=17532882
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27381089A Pending JPH03137008A (en) | 1989-10-23 | 1989-10-23 | Production of tellurium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03137008A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303879A (en) * | 2013-06-28 | 2013-09-18 | 上海应用技术学院 | Preparation method of high-purity tellurium dioxide powder |
-
1989
- 1989-10-23 JP JP27381089A patent/JPH03137008A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303879A (en) * | 2013-06-28 | 2013-09-18 | 上海应用技术学院 | Preparation method of high-purity tellurium dioxide powder |
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