JPS6356166B2 - - Google Patents
Info
- Publication number
- JPS6356166B2 JPS6356166B2 JP55058763A JP5876380A JPS6356166B2 JP S6356166 B2 JPS6356166 B2 JP S6356166B2 JP 55058763 A JP55058763 A JP 55058763A JP 5876380 A JP5876380 A JP 5876380A JP S6356166 B2 JPS6356166 B2 JP S6356166B2
- Authority
- JP
- Japan
- Prior art keywords
- suspension
- peroxide
- hydroxide
- alkaline earth
- earth metal
- 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
- 238000000034 method Methods 0.000 claims description 27
- 239000000725 suspension Substances 0.000 claims description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 15
- 239000011541 reaction mixture Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- 150000002978 peroxides Chemical class 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 6
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 4
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 3
- 239000007900 aqueous suspension Substances 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 150000004679 hydroxides Chemical class 0.000 claims 1
- 229910021450 lithium metal oxide Inorganic materials 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 239000000047 product Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 239000007921 spray Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 150000004974 alkaline earth metal peroxides Chemical class 0.000 description 4
- 235000019402 calcium peroxide Nutrition 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 229910018071 Li 2 O 2 Inorganic materials 0.000 description 2
- -1 Peroxide compounds Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004343 Calcium peroxide Substances 0.000 description 1
- 229910001323 Li2O2 Inorganic materials 0.000 description 1
- 239000003808 active oxygen stabilizer Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/04—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof
- C01B15/043—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of alkali metals, alkaline earth metals or magnesium or beryllium or aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fertilizers (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
【発明の詳細な説明】
本発明は、過酸化リチウム又はアルカリ土類金
属過酸化物の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing lithium peroxide or alkaline earth metal peroxide.
過酸化リチウム及びアルカリ土類金属過酸化物
は、工業上多量に使用される。すなわち、例えば
アルカリ土類金属過酸化物は、医学及び薬理学の
目的のために及び美容術に使用される。更に、栽
培植物の生育を改善するために使用されるので、
多量のCaO2が重要になる。また、廃水技術でも、
緩慢な酸素放出に過酸化物化合物を利用すること
ができる。 Lithium peroxide and alkaline earth metal peroxides are used in large quantities in industry. Thus, for example, alkaline earth metal peroxides are used for medical and pharmacological purposes and in cosmetology. Additionally, it is used to improve the growth of cultivated plants, so
A large amount of CaO 2 becomes important. Also, in wastewater technology,
Peroxide compounds can be utilized for slow oxygen release.
アルカリ金属及びアルカリ土類金属過酸化物
は、一般にそれらの塩、酸化物又は水酸化物の水
溶液から過酸化水素水溶液との反応によつて過酸
化物含有反応混合物を得、この混合物を遠心分離
するか又は別し、かつ乾燥台上で乾燥させるこ
とによつて製造される。この乾燥物質は、常法で
粉砕しかつ場合によつては篩別する。 Alkali metal and alkaline earth metal peroxides are generally obtained by reacting an aqueous solution of their salt, oxide or hydroxide with an aqueous hydrogen peroxide solution to obtain a peroxide-containing reaction mixture, and then centrifuging this mixture. or by separating and drying on a drying rack. This dry material is ground and optionally sieved in the customary manner.
西ドイツ国特許公開公報第1542642号の記載か
ら、CaO2の製造法が公知であり、該方法によれ
ば、著しく薄めた過酸化水物の溶液と水酸化カル
シウムの過剰量とを30℃以下の温度で反応させて
過酸化カルシウム八水和物にし、次にこの水和物
を付加的な乾燥工程で無水過酸化物に変換させ
る。 A method for producing CaO 2 is known from West German Patent Publication no. The reaction is carried out at temperature to give calcium peroxide octahydrate, which is then converted to anhydrous peroxide in an additional drying step.
全てのこれらの方法は、一連の欠点をもつ。該
方法は、遠心分離による母液の分離及び乾燥台上
で乾燥した生成物の粉砕を必要とするために費用
がかかる。更に、経済性は僅かにのみ与えられ
る。それというのも、比較的薄めた懸濁液によつ
て生じる多量の母液量中で過酸化水素を分解する
ことによつて著しい過酸化物損失をまねき、なら
びに長い滞留時間に限定される乾燥工程において
著しい過酸化物損失をまねくからである。 All these methods have a series of drawbacks. The process is expensive because it requires separation of the mother liquor by centrifugation and grinding of the dried product on a drying platform. Moreover, the economy is only marginal. This is because the decomposition of hydrogen peroxide in the large mother liquor volume produced by relatively dilute suspensions leads to significant peroxide losses, and the drying process is limited by long residence times. This is because it causes significant peroxide loss in the process.
更に、反応混合物を強く稀釈するために多量の
水を不必要に運搬しかつ大きいエネルギー消費の
乾燥工程で除去しなければならない。更に、温度
を制御するための付加的な調節装置及び水酸化カ
ルシウムの過剰量を除去するための付加的な工程
が必要である。他の欠点は、乾燥の間及び引続く
粉砕工程の間に分解することによつて得られる最
終生成物がある程度不均質であることにある。 Furthermore, due to the strong dilution of the reaction mixture, large amounts of water must be transported unnecessarily and removed in energy-consuming drying steps. Furthermore, additional regulating equipment to control the temperature and an additional step to remove excess calcium hydroxide are required. Another disadvantage lies in the degree of heterogeneity of the final product obtained by decomposition during drying and subsequent milling steps.
本発明の課題は、公知方法の欠点を回避する、
過酸化リチウム又はアルカリ土類金属過酸化物の
製造法を使用することである。 The object of the invention is to avoid the disadvantages of the known methods.
The method for producing lithium peroxide or alkaline earth metal peroxides is used.
本発明によれば、この課題を解決するために
は、200g/よりも多い酸化物含有量又は水酸
化物含有量を有する酸化リチウムもしくはアルカ
リ土類金属酸化物又は水酸化リチウムもしくはア
ルカリ土類金属水酸化物の水性懸濁液をH2O250
重量%以上の過酸化水素水溶液と混合し、引続き
噴霧乾燥させる。 According to the invention, in order to solve this problem, lithium oxide or alkaline earth metal oxides or lithium hydroxide or alkaline earth metal oxides with an oxide content or hydroxide content of more than 200 g/ Aqueous suspension of hydroxide in H 2 O 2 50
It is mixed with at least % by weight aqueous hydrogen peroxide solution and subsequently spray-dried.
意外なことに、公知方法の欠点は、できるだけ
濃厚な懸濁液を用いて作業し、この懸濁液を他の
処理過程なしに直接に注意深く乾燥させることに
よつて克服することができる。使用すべき酸化物
懸濁液もしくは水酸化物懸濁液は、高い固体含有
量を有するべきである。直接になおポンプ作用で
搬送可能な懸濁液を使用するのが最適である。こ
の場合、この懸濁液の固体含有量は、使用すべき
酸化物もしくは水酸化物により左右されるが、こ
れは通例200g/以上、有利に300g/以上で
ある。 Surprisingly, the disadvantages of the known process can be overcome by working with a suspension as thick as possible and carefully drying this suspension directly without further processing steps. The oxide or hydroxide suspensions to be used should have a high solids content. It is best to use suspensions that can be directly pumped. The solids content of the suspension in this case depends on the oxide or hydroxide to be used, but it is usually more than 200 g/, preferably more than 300 g/.
使用すべき懸濁液は、例えば水及び市販の酸化
物粉末もしくは水酸化物粉末を同時に配量するこ
とによつて撹拌下で配合物容器中で製造すること
ができる。本方法の優れた実施態様では、懸濁液
それ自身の発熱溶解工程によつて加熱された懸濁
液をそれぞれ中間冷却することなしに直接過酸化
水素と混合する。 The suspension to be used can be prepared, for example, by simultaneous metering of water and commercially available oxide or hydroxide powder in a formulation container under stirring. In a preferred embodiment of the process, the suspension, which has been heated by an exothermic dissolution step of the suspension itself, is mixed directly with the hydrogen peroxide, each without intercooling.
過酸化水素溶液としては、公知の活性酸素安定
剤を含有することもできる市販の製品を使用する
ことができる。この場合には、反応配合物をあま
り強く稀釈しない50重量%以上、有利に65重量%
以上のH2O2濃度を選択するのが望ましい。 As the hydrogen peroxide solution, commercially available products that may also contain known active oxygen stabilizers can be used. In this case, the reaction mixture should not be diluted too strongly, preferably at least 50% by weight, preferably 65% by weight.
It is desirable to select a H 2 O 2 concentration higher than or equal to the above.
本発明方法は、次のように実施することができ
る:
適当な酸化物又は水酸化物をできるだけ少ない
水量と懸濁させ、生成する酸化物−又は水酸化物
懸濁液を過酸化水素水溶液と、強力混合装置中
で、場合によつては冷却下で混合し、引続き生成
する過酸化物懸濁液を、場合によつては後冷却下
で反応が完結するまで混練機中で処理し、ペース
ト状物を噴霧乾燥機にポンプ作用で搬入し、この
噴霧乾燥機中で生成物を温風流中の回転式円板上
で粉末状にする。 The process according to the invention can be carried out as follows: A suitable oxide or hydroxide is suspended in as little water as possible and the resulting oxide-or hydroxide suspension is mixed with an aqueous hydrogen peroxide solution. , in an intensive mixer, optionally with cooling, and subsequently treating the resulting peroxide suspension in a kneader until the reaction is complete, optionally with post-cooling, The paste is pumped into a spray dryer in which the product is pulverized on a rotating disk in a stream of hot air.
強力混合装置としては、例えば高速回転型偏心
ポンプ又は場合によつては冷却ジヤケツトを備え
る鋤形ミキサーを使用することができる。反応成
分を合しかつ混合した後、有利に反応混合物に対
して水含有量が約40重量%になるまで反応混合物
から水含有量の一部を取り去るのが有利である。
反応が完結するまで反応混合物を処理するため
に、例えば円錐形スクリユーミキサーを使用する
ことができる。このミキサー中で、反応混合物は
3時間まで、有利に0.5時間まで、すなわち反応
が完結するまでもしくは変換度が最適になるまで
混練することができる。ペースト状物は、本発明
方法ではスクリユーポンプを用いて運搬すること
ができる。反応生成物を乾燥するには、高速回転
式円板を有する噴霧乾燥機が好適であることが判
明する。 As intensive mixing devices it is possible to use, for example, high-speed eccentric pumps or spade mixers, if appropriate with cooling jackets. After the reaction components have been combined and mixed, it is advantageous to remove part of the water content from the reaction mixture, preferably until the water content is about 40% by weight, based on the reaction mixture.
For example, a conical screw mixer can be used to process the reaction mixture until the reaction is complete. In this mixer, the reaction mixture can be kneaded for up to 3 hours, preferably for up to 0.5 hours, ie until the reaction is complete or the degree of conversion is optimum. The paste can be conveyed in the method according to the invention using a screw pump. Spray dryers with high speed rotating discs have proven suitable for drying the reaction products.
本発明方法は、公知技術に比べて次の利点を有
する:
a 反応成分をほぼ化学量論的に使用すること及
び濃厚な反応混合物で作業することによつて、
一緒に移動すべきバラスト(水、過剰の反応成
分)の含分は最低量で保持される。 The process of the invention has the following advantages over the known technology: a. By using the reaction components approximately stoichiometrically and by working with concentrated reaction mixtures,
The content of ballast (water, excess reaction components) to be transferred is kept to a minimum.
b 反応混合物に直接噴霧乾燥することによつ
て、費用のかかる分離工程及び浄化工程は省略
される。更に、生成物は、自由に流動する顆粒
として直接に沈殿し、かつ付加的に粉砕装置中
で最終的に処理する必要はない。b By spray drying directly onto the reaction mixture, expensive separation and purification steps are omitted. Furthermore, the product is precipitated directly as free-flowing granules and does not additionally need to be further processed in a milling device.
c 本方法は、不連続的にも実施することができ
る。c The method can also be carried out discontinuously.
また、本発明方法により得られる生成物も公知
技術のものに比べて次の利点を有する:
a 局所的な分解反応を回避することは、生成物
の良好な均一性を保証する。 The products obtained by the process of the invention also have the following advantages compared to those of the prior art: a Avoiding local decomposition reactions ensures good homogeneity of the products.
b 噴霧乾燥することによつて、良好な流動性、
均一の結晶構造及び単一で狭い粒子スペクトル
が達成される。b good fluidity by spray drying;
A uniform crystal structure and a single, narrow grain spectrum are achieved.
c 強力乾燥することによつてのみ、結晶水不含
の過酸化物が得られる。c Only by intensive drying can a peroxide free of water of crystallization be obtained.
本発明方法を第1図の略図につき詳説する。1
は酸化物懸濁液又は水酸化物懸濁液を製造する混
合装置を示し、2中にはH2O2溶液が用意されて
いる。装入溶液を強力混合装置3中で合し、これ
を冷却器4を介して円錐形スクリユーミキサー5
に導入する。5中での滞留時間は、実施態様に応
じて3時間まで、有利に0.5時間までであること
ができる。反応生成物を、スクリユーポンプ6に
よつて連続的に5から取り出し、かつ噴霧乾燥す
るために噴霧乾燥機7に導く。本発明方法の詳細
を実施態様では、反応混合物の一部を、冷却器4
に侵入する前にバイパス8を介して取り去り、か
つ迅速な反応開始のために混合装置3中に戻すこ
とができる。混合装置1及び3は、付加的に冷却
装置を備えていてもよい。 The method according to the invention will be explained in more detail with reference to the schematic diagram in FIG. 1
2 shows a mixing device for producing an oxide suspension or a hydroxide suspension, in which a H 2 O 2 solution is prepared. The starting solutions are combined in an intensive mixer 3 and passed through a condenser 4 to a conical screw mixer 5.
to be introduced. Depending on the embodiment, the residence time in 5 can be up to 3 hours, preferably up to 0.5 hours. The reaction product is continuously removed from 5 by means of a screw pump 6 and led to a spray dryer 7 for spray drying. In a detailed embodiment of the method of the invention, a portion of the reaction mixture is transferred to a cooler 4.
can be removed via a bypass 8 before entering the reactor and returned to the mixing device 3 for rapid reaction initiation. Mixing devices 1 and 3 may additionally be equipped with a cooling device.
本発明方法を次の実施例につき詳説するが、本
発明はこれによつて限定されるものではない。 The method of the invention will be explained in detail with reference to the following examples, but the invention is not limited thereby.
例 1
配合物容器1中で、水及びCa(OH2)2粉末を同
時に配量することによつて、Ca(OH)250重量%
を含有するCa(OH)2懸濁液を撹拌下で得る。貯
蔵容器2中に、PO3 4 -300g/で安定化された70
重量%のH2O2水溶液を用意する。スクリユーポ
ンプを用いての1からの毎時Ca(OH)2懸濁液660
Kgとピストン配量ポンプを用いての2からの毎時
H2O2溶液186とを反応させ、この反応混合物を
高速ミキサーポンプ(スプラトン(Supraton
)
207)3に貫流する。この方法で、熱発生下で毎
時CaO2スラリー900Kgが形成される。Example 1 50% by weight of Ca(OH) 2 by simultaneously metering water and Ca(OH 2 ) 2 powder in formulation container 1
A Ca(OH) 2 suspension containing is obtained under stirring. In storage container 2, 70 stabilized with PO 3 4 - 300 g/
Prepare a wt% H2O2 aqueous solution . Ca(OH) 2 suspension per hour from 1660 using screw pump
Kg and hourly from 2 using piston metering pump
H 2 O 2 solution 186 and the reaction mixture was pumped into a high speed mixer pump (Supraton).
207) Flows through 3. In this way, 900Kg of CaO 2 slurry is formed per hour under heat generation.
このスラリーを、(垂直に配置され、水で冷却
されたダブルシリンダー中で、冷却すべきスラリ
ーを撹拌機を用いて冷却面で遠心分離し、この遠
心分離されたスラリーを、次に冷却し、下方に流
出させる)薄層熱交換器4中で308Kに冷却し、
かつ該交換器から易流動性でスクリユーミキサー
5中に流入させる。 This slurry is then cooled (in a double cylinder arranged vertically and cooled with water, the slurry to be cooled is centrifuged on a cooling surface using a stirrer; this centrifuged slurry is then cooled; cooled to 308 K in a thin layer heat exchanger 4 (flowing downward),
From the exchanger it flows freely into the screw mixer 5.
CaO2スラリーを該ミキサーからスクリユーポ
ンプ6を用いて乾燥するために噴霧乾燥機7上に
供給する。乾燥温度は、不断の生成物流に合わせ
て調節され、乾燥機の入口で473K、乾燥機の出
口で348Kである。こうして得られる生成物(毎
時324Kg)は、CaO276.4重量%を含有する。
REM撮影(第2図)から、平均粒径は5μであり、
粒子の約90%は直径2〜7μを有することを知る
ことができる。H2O2に対するMgO2の収率64.2
%。 The CaO2 slurry is fed from the mixer onto a spray dryer 7 for drying using a screw pump 6. The drying temperature is adjusted to the constant product flow and is 473 K at the dryer inlet and 348 K at the dryer outlet. The product thus obtained (324 Kg/h) contains 76.4% by weight of CaO 2 .
From REM photography (Figure 2), the average particle size is 5μ,
It can be seen that approximately 90% of the particles have a diameter of 2-7μ. Yield of MgO2 relative to H2O2 64.2
%.
例 2
例1に記載した作業法と同様にして、25重量%
のMgO懸濁液毎時496Kgと70重量%のH2O2溶液
毎時60とを反応させて貫流する。Example 2 Using the same method as described in Example 1, 25% by weight
496Kg of MgO suspension per hour is reacted with 60Kg of 70% by weight H2O2 solution per hour.
ミキサーポンプの、部分流(30容量%)をバイ
パス8を介して迅速な反応開始のためにミキサー
ポンプ中に戻し;MgO2−スラリー(毎時573Kg)
を、例1の記載と同様にして冷却し、スクリユー
ミキサー中に中間貯蔵し、かつ噴霧乾燥機中で乾
燥させる。 A partial stream (30% by volume) of the mixer pump is returned via bypass 8 into the mixer pump for rapid reaction initiation; MgO 2 -slurry (573 Kg/h)
is cooled as described in Example 1, intermediately stored in a screw mixer and dried in a spray dryer.
こうして得られる生成物(毎時122Kg)は、
MgO245.8重量%を含有する。 The product thus obtained (122Kg/hour) is
Contains 45.8% by weight of MgO2 .
例 3
例1に記載した作業法と同様にして、41重量%
のLiOH懸濁液毎時132Kgと70重量%のH2O2溶液
毎時47とを反応させて貫流する。この方法で、
熱発生下でLi2O2−スラリー毎時193Kgが形成さ
れる。Example 3 Using the same method as described in Example 1, 41% by weight
132Kg of LiOH suspension per hour is reacted with 47Kg of 70% by weight H 2 O 2 solution per hour. using this method,
Under heat generation, 193 Kg of Li 2 O 2 -slurry is formed per hour.
例1により後処理すると、Li2O289%を含有す
る生成物(毎時52Kg)が得られる。H2O2に対す
るLi2O2の収率83.3%。 After working up according to Example 1, a product containing 89% Li 2 O 2 (52 Kg/h) is obtained. Yield of Li2O2 relative to H2O2 83.3%.
例 4
別法で、例1により製造されたCaO2スラリー
をミキサーポンプからデカンター中に供給し、該
デカンター中で該スラリーを全水含有量が約40重
量%になるまで脱水する。該デカンターから該ス
ラリーをスクリユーポンプに供給し、該スクリユ
ーポンプは噴霧円板を有する噴霧乾燥機に濃厚ス
ラリーを供給する。この直接加熱された噴霧乾燥
機中で、スラリーを吸気温度約773K及び排気温
度約383Kで乾燥させる。Example 4 Alternatively, the CaO 2 slurry produced according to Example 1 is fed from a mixer pump into a decanter in which the slurry is dewatered to a total water content of about 40% by weight. The decanter feeds the slurry to a screw pump which feeds the thick slurry to a spray dryer having a spray disk. The slurry is dried in this directly heated spray dryer at an inlet temperature of about 773K and an exhaust temperature of about 383K.
該乾燥機を離れる粉末状で易流動性の乾燥生成
物は、CaO275重量%を含有し、実際に結晶水を
含有せず、かつ冷却後、粉砕することなしに直接
貯蔵することができるかあるいは包装することが
できる。H2O2に対するCaO2の収率67.7%。 The powdery, free-flowing dry product leaving the dryer contains 75% by weight of CaO2 , practically contains no water of crystallization, and after cooling can be stored directly without grinding. or can be packaged. Yield of CaO2 relative to H2O2 67.7%.
強調すべきことは、工業的品質のCa(OH)2を
使用するにも拘らず良好な安定度の製品が得ら
れ、この製品は普通の貯蔵条件下で1ケ月間より
大きい活性酸素損失なしに貯蔵することができる
ことである。 It should be emphasized that, despite using industrial quality Ca(OH) 2 , a product of good stability was obtained, which under normal storage conditions had no active oxygen loss greater than 1 month. It can be stored in
第1図は、本発明の方法を実施する装置の略示
系統図であり、第2図は、本発明の方法により得
られる生成物を示す、REM撮影による電子顕微
鏡写真(倍率1000×)である。
1……混合装置、2……貯蔵容器、3……強力
混合装置、4……冷却器、5……円錐形スクリユ
ーミキサー、6……スクリユーポンプ、7……噴
霧乾燥機、8……バイパス。
FIG. 1 is a schematic diagram of an apparatus for carrying out the method of the present invention, and FIG. 2 is an electron micrograph (magnification: 1000×) obtained by REM photography showing the product obtained by the method of the present invention. be. 1... Mixing device, 2... Storage container, 3... Strong mixing device, 4... Cooler, 5... Conical screw mixer, 6... Screw pump, 7... Spray dryer, 8... …bypass.
Claims (1)
水酸化物を過酸化水素と反応させることによつて
過酸化リチウム又はアルカリ土類金属過酸化物を
製造する方法において、200g/よりも多い酸
化物含有量又は水酸化物含有量を有する酸化物又
は水酸化物の水性懸濁液をH2O250重量%以上の
過酸化水素水溶液と混合し、引続き噴霧乾燥させ
ることを特徴とする、過酸化リチウム又はアルカ
リ土類金属過酸化物の製造法。 2 酸化物懸濁液又は水酸化物懸濁液は、なおポ
ンプ作用で搬送可能であるような程度の高さの固
体含有量を有する、特許請求の範囲第1項記載の
方法。 3 酸化物懸濁液又は水酸化物懸濁液の固体含有
量は、300g/より多い、特許請求の範囲第1
項又は第2項に記載の方法。 4 反応成分を化学量論的量で合する、特許請求
の範囲第1項から第3項までのいずれか1項に記
載の方法。 5 過酸化物懸濁液を3時間まで熟成させる、特
許請求の範囲第1項から第4項までのいずれか1
項に記載の方法。 6 アルカリ土類金属としてマグネシウム又はカ
ルシウムを選択する、特許請求の範囲第1項から
第5項までのいずれか1項に記載の方法。 7 混合工程を離れた後の反応混合物の一部をそ
の混合工程に戻す、特許請求の範囲第1項から第
6項までのいずれか1項に記載の方法。 8 反応成分を合しかつ混合した後、反応混合物
から、反応混合物に対して水含有量が40重量%に
なるまで水含有量の一部を取り去る、特許請求の
範囲第1項から第7項までのいずれか1項に記載
の方法。[Scope of Claims] 1. A method for producing lithium peroxide or alkaline earth metal peroxide by reacting lithium or alkaline earth metal oxide or hydroxide with hydrogen peroxide, An aqueous suspension of oxides or hydroxides having an oxide content or a hydroxide content of more than A method for producing lithium peroxide or alkaline earth metal peroxide, characterized by: 2. Process according to claim 1, characterized in that the oxide suspension or hydroxide suspension has such a high solids content that it can still be pumped. 3. The solids content of the oxide suspension or hydroxide suspension is greater than 300 g/Claim 1.
or the method described in paragraph 2. 4. A process according to any one of claims 1 to 3, wherein the reaction components are combined in stoichiometric amounts. 5. Any one of claims 1 to 4, wherein the peroxide suspension is aged for up to 3 hours.
The method described in section. 6. The method according to any one of claims 1 to 5, wherein magnesium or calcium is selected as the alkaline earth metal. 7. The method according to any one of claims 1 to 6, wherein a portion of the reaction mixture after leaving the mixing step is returned to the mixing step. 8. After combining and mixing the reaction components, a portion of the water content is removed from the reaction mixture until the water content is 40% by weight relative to the reaction mixture, as claimed in claims 1 to 7. The method described in any one of the above.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19792918137 DE2918137A1 (en) | 1979-05-05 | 1979-05-05 | METHOD FOR PRODUCING ALKALINE OR ALKALINE EARTH PEROXIDES |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS55149107A JPS55149107A (en) | 1980-11-20 |
JPS6356166B2 true JPS6356166B2 (en) | 1988-11-07 |
Family
ID=6069996
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP5876380A Granted JPS55149107A (en) | 1979-05-05 | 1980-05-06 | Preparation of alkali metal or alkaline earth metal peroxide |
Country Status (13)
Country | Link |
---|---|
JP (1) | JPS55149107A (en) |
AT (1) | AT382139B (en) |
AU (1) | AU541584B2 (en) |
BE (1) | BE883079A (en) |
BR (1) | BR8002696A (en) |
CA (1) | CA1167235A (en) |
DE (1) | DE2918137A1 (en) |
ES (1) | ES489620A1 (en) |
FR (1) | FR2456069B1 (en) |
GB (1) | GB2048842B (en) |
IT (1) | IT1140860B (en) |
LU (1) | LU82328A1 (en) |
NL (1) | NL189083C (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02120478U (en) * | 1989-03-17 | 1990-09-28 |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ATE7012T1 (en) * | 1980-05-15 | 1984-04-15 | Interox Chemicals Limited | PRODUCTION OF ALKALINE OR ALKALI-EARTH METAL PEROXIDES AND PEROXIDES SO MANUFACTURED. |
DE3025682A1 (en) * | 1980-07-07 | 1982-02-11 | Peroxid-Chemie GmbH, 8023 Höllriegelskreuth | METHOD FOR PRODUCING PEROXIDES OF TWO-VALUE METALS |
JPS5773607A (en) * | 1980-10-24 | 1982-05-08 | Dainippon Printing Co Ltd | Calibration system of lithographic-plate pattern area rate meter |
DE3105584A1 (en) * | 1981-02-16 | 1982-10-28 | Peroxid-Chemie GmbH, 8023 Höllriegelskreuth | METHOD FOR CONTINUOUSLY DETERMINING ALKALI HYPEROXIDE |
US5186165A (en) * | 1991-06-05 | 1993-02-16 | Brookdale International Systems Inc. | Filtering canister with deployable hood and mouthpiece |
US5394867A (en) * | 1991-06-05 | 1995-03-07 | Brookdale International Systems Inc. | Personal disposable emergency breathing system with dual air supply |
DE4219459A1 (en) * | 1992-06-13 | 1993-12-16 | Huels Chemische Werke Ag | Process for the preparation of 2,2,6,6-tetramethylpiperidine-N-oxyl and its derivatives substituted in the 4-position |
DE19650686A1 (en) * | 1996-12-06 | 1998-06-10 | Solvay Interox Gmbh | Alkaline earth metal peroxide product |
DE10035287A1 (en) | 2000-07-18 | 2002-01-31 | Solvay Interox Gmbh | Coated metal peroxides |
DE10248652A1 (en) | 2002-10-18 | 2004-04-29 | Solvay Interox Gmbh | Process for the production of dust-free alkaline earth peroxides |
WO2007098629A1 (en) * | 2006-02-28 | 2007-09-07 | Swissdent Cosmetics Ag | Toothpaste |
CN114634165B (en) * | 2022-01-20 | 2023-08-29 | 常熟理工学院 | Method for preparing calcium peroxide by utilizing waste incineration fly ash |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3134646A (en) * | 1962-01-15 | 1964-05-26 | Lithium Corp | Preparation of lithium peroxide |
JPS4970896A (en) * | 1972-11-10 | 1974-07-09 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2415443A (en) * | 1944-11-28 | 1947-02-11 | Albert Pavlik | Strontium peroxide and method of making the same |
US2695217A (en) * | 1952-05-22 | 1954-11-23 | Shell Dev | Purification of hydrogen peroxide |
US3120997A (en) * | 1961-08-25 | 1964-02-11 | Gen Dynamics Corp | Process for producing alkali metal superoxides |
US3446588A (en) * | 1967-03-02 | 1969-05-27 | Foote Mineral Co | Method for preparing lithium peroxide |
JPS5039078B1 (en) * | 1971-02-22 | 1975-12-13 | ||
FR2175652B1 (en) * | 1972-03-17 | 1974-08-02 | Air Liquide | |
US3907506A (en) * | 1972-03-17 | 1975-09-23 | Air Liquide | Apparatus for the preparation of alkaline hyperoxide |
-
1979
- 1979-05-05 DE DE19792918137 patent/DE2918137A1/en active Granted
-
1980
- 1980-03-03 NL NLAANVRAGE8001274,A patent/NL189083C/en not_active IP Right Cessation
- 1980-03-17 ES ES489620A patent/ES489620A1/en not_active Expired
- 1980-04-03 LU LU82328A patent/LU82328A1/en unknown
- 1980-04-15 IT IT21372/80A patent/IT1140860B/en active
- 1980-04-17 AU AU57553/80A patent/AU541584B2/en not_active Expired - Fee Related
- 1980-04-29 GB GB8014089A patent/GB2048842B/en not_active Expired
- 1980-04-30 BR BR8002696A patent/BR8002696A/en not_active IP Right Cessation
- 1980-05-02 BE BE1/9804A patent/BE883079A/en not_active IP Right Cessation
- 1980-05-05 CA CA000351249A patent/CA1167235A/en not_active Expired
- 1980-05-05 AT AT0238280A patent/AT382139B/en not_active IP Right Cessation
- 1980-05-05 FR FR8010024A patent/FR2456069B1/en not_active Expired
- 1980-05-06 JP JP5876380A patent/JPS55149107A/en active Granted
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3134646A (en) * | 1962-01-15 | 1964-05-26 | Lithium Corp | Preparation of lithium peroxide |
JPS4970896A (en) * | 1972-11-10 | 1974-07-09 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02120478U (en) * | 1989-03-17 | 1990-09-28 |
Also Published As
Publication number | Publication date |
---|---|
AU5755380A (en) | 1980-11-13 |
DE2918137C2 (en) | 1988-06-09 |
DE2918137A1 (en) | 1980-11-20 |
FR2456069B1 (en) | 1985-10-11 |
JPS55149107A (en) | 1980-11-20 |
GB2048842B (en) | 1983-02-23 |
IT1140860B (en) | 1986-10-10 |
BR8002696A (en) | 1980-12-16 |
FR2456069A1 (en) | 1980-12-05 |
IT8021372A0 (en) | 1980-04-15 |
ATA238280A (en) | 1986-06-15 |
ES489620A1 (en) | 1980-09-16 |
CA1167235A (en) | 1984-05-15 |
NL8001274A (en) | 1980-11-07 |
BE883079A (en) | 1980-11-03 |
AT382139B (en) | 1987-01-12 |
GB2048842A (en) | 1980-12-17 |
NL189083C (en) | 1993-01-04 |
NL189083B (en) | 1992-08-03 |
AU541584B2 (en) | 1985-01-10 |
LU82328A1 (en) | 1980-07-02 |
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