JPH08245204A - Refining method of hydrogen peroxide aqueous solution - Google Patents
Refining method of hydrogen peroxide aqueous solutionInfo
- Publication number
- JPH08245204A JPH08245204A JP4853595A JP4853595A JPH08245204A JP H08245204 A JPH08245204 A JP H08245204A JP 4853595 A JP4853595 A JP 4853595A JP 4853595 A JP4853595 A JP 4853595A JP H08245204 A JPH08245204 A JP H08245204A
- Authority
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- Japan
- Prior art keywords
- hydrogen peroxide
- exchange resin
- solid phase
- aqueous solution
- impurities
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、無機不純物及び有機不
純物を含む不純過酸化水素水溶液を精製し、何れの不純
物も微量にしか含まない極めて高純度な過酸化水素水溶
液を得る方法に関する。本発明により精製された過酸化
水素水溶液は主に半導体製造分野で使用される。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for purifying an impure hydrogen peroxide aqueous solution containing inorganic impurities and organic impurities to obtain an extremely high purity hydrogen peroxide aqueous solution containing only a trace amount of each impurity. The hydrogen peroxide aqueous solution purified according to the present invention is mainly used in the field of semiconductor manufacturing.
【０００２】[0002]
【従来の技術】現在、過酸化水素水溶液は主にアントラ
キノン類の自動酸化法により製造されている。この方法
により製造された過酸化水素水溶液は、一般に、製造装
置や貯蔵装置からの溶出又は安定剤の添加などによっ
て、約５ｐｐｂ〜約１０ｐｐｍ程度の種々の金属カチオ
ン、約１０ｐｐｂ〜約１０ｐｐｍ程度の種々のアニオ
ン、さらには、アントラキノン類、溶媒またはそれらの
変質物の混入などにより全有機炭素量（ＴＯＣ）として
約１０ｍｇ／Ｌ〜数百ｍｇ／Ｌ程度の有機不純物を含有
している。2. Description of the Related Art At present, an aqueous hydrogen peroxide solution is mainly produced by an autoxidation method of anthraquinones. The aqueous solution of hydrogen peroxide produced by this method generally contains various metal cations of about 5 ppb to about 10 ppm and various metal cations of about 10 ppb to about 10 ppm due to elution from a production apparatus or storage apparatus or addition of a stabilizer. And further contains an organic impurity of about 10 mg / L to several hundreds mg / L as the total amount of organic carbon (TOC) due to the inclusion of anthraquinones, solvents or their modified substances.
【０００３】[0003]
【発明が解決しようとする問題点】過酸化水素水溶液は
従来反応試剤、漂白、化学研磨などの分野で広く利用さ
れてきたが、近年、半導体製造の分野でウェハーの洗
浄、エッチングなどへの利用が増大している。この分野
では極めて高純度の過酸化水素水溶液が要求されてお
り、前述した不純物を除去する必要がある。本発明の目
的は、極めて高品質の精製された過酸化水素水溶液を工
業的に安全に製造する方法を提供することにある。The aqueous hydrogen peroxide solution has been widely used in the fields of reaction reagents, bleaching, chemical polishing, etc., but in recent years, it has been used for cleaning and etching wafers in the field of semiconductor manufacturing. Is increasing. In this field, an extremely high-purity hydrogen peroxide aqueous solution is required, and it is necessary to remove the above-mentioned impurities. An object of the present invention is to provide a method for industrially safely producing an extremely high-quality purified hydrogen peroxide aqueous solution.
【０００４】[0004]
【問題点を解決するための手段】本発明者らは、前記の
目的を達成するべく鋭意検討し、本発明を完成するに至
った。本発明の特徴は、過酸化水素水溶液を精製するに
際し、原料過酸化水素水溶液を冷却して固相を析出さ
せ、次いで、互いに異なる少なくとも２種のイオン交換
樹脂層に通液せしめる点にある。[Means for Solving the Problems] The inventors of the present invention have conducted extensive studies to achieve the above-mentioned object, and completed the present invention. A feature of the present invention is that when purifying an aqueous solution of hydrogen peroxide, the aqueous solution of hydrogen peroxide as a raw material is cooled to precipitate a solid phase, and then the solution is passed through at least two kinds of ion exchange resin layers different from each other.
【０００５】本発明においては、４５．２重量％以上の
濃度の過酸化水素水溶液が使用できる。特に、４５．２
重量％以上であって６１重量％以下好ましくは６０重量
％未満の濃度を有する過酸化水素水溶液は、入手し易く
取扱いも容易である上に、これを原料にして冷却する
と、過酸化水素を４８．６重量％含有する過酸化水素水
和物結晶からなる固相が生成する。このような過酸化水
素濃度を有する固相は、融解後の取扱いも容易であるの
で工業的な実施に適している。一方、４５．２重量％未
満の過酸化水素水溶液を冷却すると、水が固相として分
離し、過酸化水素水溶液の精製には効果が無い。In the present invention, an aqueous hydrogen peroxide solution having a concentration of 45.2% by weight or more can be used. In particular, 45.2
An aqueous solution of hydrogen peroxide having a concentration of not less than 61% by weight and preferably not more than 60% by weight is easily available and easy to handle, and when it is used as a raw material and cooled, hydrogen peroxide is reduced to 48%. A solid phase consisting of hydrogen peroxide hydrate crystals containing 0.6% by weight is formed. A solid phase having such a hydrogen peroxide concentration is easy to handle after melting, and is suitable for industrial use. On the other hand, when the aqueous hydrogen peroxide solution of less than 45.2% by weight is cooled, water is separated as a solid phase, which has no effect on the purification of the aqueous hydrogen peroxide solution.
【０００６】冷却槽の材質は、アルミニウムまたはSUS3
04、SUS316などのステンレスが好ましい。The material of the cooling tank is aluminum or SUS3
04, stainless steel such as SUS316 is preferable.
【０００７】本発明における固相の析出、回収、融解操
作は、回分式でも連続式でも可能である。固相の成長速
度は小さいことが好ましい。固相の析出を行う際には、
種結晶として過酸化水素または過酸化水素水和物の結晶
を少量添加することが好ましい。The solid phase precipitation, recovery and melting operations in the present invention can be carried out batchwise or continuously. The solid phase growth rate is preferably low. When performing solid phase precipitation,
It is preferable to add a small amount of hydrogen peroxide or hydrogen peroxide hydrate crystals as seed crystals.
【０００８】固相の析出時には種結晶を添加することが
好ましい。特に、冷却槽内の原料過酸化水素水溶液の温
度が、その過酸化水素水溶液濃度における凝固点温度よ
りも２℃以内の温度差で低い温度にある状態で、種結晶
を添加することが好ましい。種結晶としては、固化した
過酸化水素水溶液が使用され、本発明の方法により精製
された過酸化水素水溶液からなる結晶を使用することが
好ましい。It is preferable to add a seed crystal during the precipitation of the solid phase. Particularly, it is preferable to add the seed crystal in a state where the temperature of the raw material hydrogen peroxide solution in the cooling tank is lower than the freezing point temperature at the hydrogen peroxide solution concentration by a temperature difference of 2 ° C. or less. As the seed crystal, a solidified hydrogen peroxide aqueous solution is used, and it is preferable to use a crystal composed of the hydrogen peroxide aqueous solution purified by the method of the present invention.
【０００９】また、連続式の場合は、冷却槽から固相を
液相とともにスラリーとして抜き出し、これを遠心脱水
することにより液相の付着の少ない固相を回収する一
方、抜き出した量に相当する量の原料過酸化水素水溶液
を冷却槽に供給することにより行われる。固相の回収量
は原料過酸化水素水溶液量の３〜４０重量％とすること
が好ましく、２０〜３５重量％とすることがより好まし
い。固相の回収量を上げようとすると、固相が容器壁や
攪拌翼に固着して固相を取り出す際の操作性が低下す
る。固相の回収量が低すぎると、操作一回当たりの精製
された過酸化水素水溶液の収量が低く、工業的な見地か
らの生産性が低い。Further, in the case of the continuous system, the solid phase is extracted from the cooling tank together with the liquid phase as a slurry, and the solid phase having less adherence of the liquid phase is recovered by centrifugal dehydration, which corresponds to the extracted amount. It is carried out by supplying the raw material hydrogen peroxide solution in an amount to the cooling tank. The recovery amount of the solid phase is preferably 3 to 40% by weight, more preferably 20 to 35% by weight of the raw material hydrogen peroxide aqueous solution. If it is attempted to increase the recovery amount of the solid phase, the solid phase adheres to the container wall or the stirring blade, and the operability at the time of taking out the solid phase deteriorates. If the recovery amount of the solid phase is too low, the yield of the purified hydrogen peroxide aqueous solution per operation will be low, and the productivity from the industrial viewpoint will be low.
【００１０】固相が析出し始めてから固相を取り出すま
での時間、すなわち、固相の析出時間は３〜１６時間が
好ましい。析出時間がこの範囲より短いと精製効率が低
く、この時間より長くても精製効率が低下する。固相の
取り出しは、固相を含む過酸化水素水溶液スラリーの濾
過又は固相を含む過酸化水素水溶液スラリーから液相を
抜き出すことにより行われる。The time from the beginning of the precipitation of the solid phase to the extraction of the solid phase, that is, the precipitation time of the solid phase is preferably 3 to 16 hours. If the precipitation time is shorter than this range, the purification efficiency will be low, and if it is longer than this time, the purification efficiency will be low. The extraction of the solid phase is performed by filtering the hydrogen peroxide aqueous solution slurry containing the solid phase or by extracting the liquid phase from the hydrogen peroxide aqueous solution slurry containing the solid phase.
【００１１】取り出された固相に付着している液相には
不純物が濃縮されているので、取り出された固相から液
相を十分に分離することが好ましい。液相の分離には遠
心脱水器が好適に使用される。固相からの液相の分離操
作においては、不純物の少ない過酸化水素水溶液により
固相を洗浄する操作や固相の一部を融解させる操作を組
み合わせることが好ましい。Since impurities are concentrated in the liquid phase adhering to the extracted solid phase, it is preferable to sufficiently separate the liquid phase from the extracted solid phase. A centrifugal dehydrator is preferably used for separating the liquid phase. In the operation of separating the liquid phase from the solid phase, it is preferable to combine an operation of washing the solid phase with an aqueous solution of hydrogen peroxide containing less impurities and an operation of melting a part of the solid phase.
【００１２】回収された固相は、これを熱交換器などを
使用して融解して液化させる。以上の冷却、固相の回
収、融解操作を２回以上繰り返してもよい。The recovered solid phase is melted and liquefied by using a heat exchanger or the like. The above cooling, solid phase recovery, and melting operations may be repeated twice or more.
【００１３】得られた過酸化水素水溶液は、好ましくは
希釈した後、カチオン交換樹脂層、アニオン交換樹脂層
及びカチオン交換樹脂とアニオン交換樹脂との混合層か
らなる群から選ばれた少なくとも２種の互いに異なる層
に通液せしめる。希釈は過酸化水素濃度が２０〜４０重
量％となるようにするのが好ましい。The obtained aqueous hydrogen peroxide solution is preferably diluted and then at least two kinds selected from the group consisting of a cation exchange resin layer, an anion exchange resin layer and a mixed layer of a cation exchange resin and an anion exchange resin. Let the liquid flow through different layers. The dilution is preferably performed so that the hydrogen peroxide concentration is 20 to 40% by weight.
【００１４】カチオン交換樹脂としては強酸性で且つ架
橋性の高いカチオン交換樹脂が好ましく、イオン交換基
としてＳＯ3Ｈ基を有する樹脂が特に好ましい。アニオ
ン交換樹脂としては強塩基性で且つ架橋性の高いアニオ
ン交換樹脂が好ましく、炭酸塩化または重炭酸塩化した
第４級アンモニウム基を有する樹脂が特に好ましい。カ
チオン交換樹脂とアニオン交換樹脂との混合層を使用す
る場合は、両者の重量比が３：９７〜９７：３となる量
を混合してこれを使用すれば良い。As the cation exchange resin, a cation exchange resin having strong acidity and high crosslinkability is preferable, and a resin having an SO 3 H group as an ion exchange group is particularly preferable. As the anion exchange resin, a strong basic and highly crosslinkable anion exchange resin is preferable, and a carbonated or bicarbonated quaternary ammonium group-containing resin is particularly preferable. When a mixed layer of a cation exchange resin and an anion exchange resin is used, the weight ratio of the both may be mixed to be used in an amount of 3:97 to 97: 3.
【００１５】本発明において、カチオン交換樹脂層、ア
ニオン交換樹脂層及びカチオン交換樹脂とアニオン交換
樹脂との混合層からなる群から選ばれた少なくとも２種
の互いに異種の層の配列順序に制限は無いが、好ましく
は、カチオン交換樹脂層次いでアニオン交換樹脂層の
順、又は、カチオン交換樹脂層、アニオン交換樹脂層次
いでカチオン交換樹脂とアニオン交換樹脂との混合層の
順である。In the present invention, there is no limitation on the arrangement order of at least two different kinds of layers selected from the group consisting of a cation exchange resin layer, an anion exchange resin layer and a mixed layer of a cation exchange resin and an anion exchange resin. However, the order is preferably cation exchange resin layer and then anion exchange resin layer, or cation exchange resin layer, anion exchange resin layer and then mixed layer of cation exchange resin and anion exchange resin.
【００１６】本発明の特徴は、原料過酸化水素水溶液を
冷却して固相を析出させた後、前記のイオン交換樹脂層
に通液せしめる点にある。これを逆にして、イオン交換
樹脂層に通液せしめた後、冷却して固相を析出させるの
では、金属の溶出のない装置を使用しても得られた過酸
化水素水溶液の精製度が低下する。本発明のような順序
とすることによってのみ、精製度が向上するのである。A feature of the present invention is that the raw material hydrogen peroxide aqueous solution is cooled to precipitate a solid phase, and then the solution is passed through the ion exchange resin layer. By reversing this and letting the solution pass through the ion exchange resin layer, and then cooling to precipitate the solid phase, the degree of purification of the obtained hydrogen peroxide aqueous solution can be improved even by using a device that does not elute metal. descend. Only by adopting the order as in the present invention, the degree of purification is improved.
【００１７】本発明の方法によれば、ＴＯＣが１ｍｇ／
Ｌ以下、いずれの金属カチオンも０．５ｐｐｂ以下、い
ずれのアニオンも１０ｐｐｂ以下にまで低下した、高純
度の過酸化水素水溶液を工業的に安全に得ることができ
る。According to the method of the present invention, TOC is 1 mg /
It is possible to industrially safely obtain a highly pure aqueous hydrogen peroxide solution having L or less, 0.5 ppb or less for all metal cations and 10 ppb or less for all anions.
【００１８】[0018]
【実施例】以下に本発明の実施例及び比較例を示すが、
本発明はこれらの実施例により限定されるものではな
い。なお、金属系の不純物の測定は、Ｃａはフレームレ
ス原子吸光法、それ以外はＩＣＰ−ＭＳ（Inductively
coupled plasma - Mass spectrometry）法による。アニ
オン性不純物はイオンクロマト法によって測定した。有
機不純物は全有機体炭素計を用いて全有機炭素量として
測定した。なお、原料及び対照例１の過酸化水素水溶液
中の不純物は、精製水で３１重量％に希釈して測定・評
価した。EXAMPLES Examples and comparative examples of the present invention will be shown below.
The invention is not limited by these examples. In addition, the measurement of metal-based impurities is carried out by a flameless atomic absorption method for Ca, and ICP-MS (Inductively
coupled plasma-Mass spectrometry) method. Anionic impurities were measured by the ion chromatography method. Organic impurities were measured as the total organic carbon content using a total organic carbon meter. Impurities in the raw material and the hydrogen peroxide aqueous solution of Comparative Example 1 were measured and evaluated by diluting them with purified water to 31% by weight.
【００１９】実施例１ 内容積２Ｌのステンレス製容器の中に、過酸化水素を５
５重量％含有する過酸化水素水溶液２２００ｇを原料と
して入れ、攪拌しながら水溶液を−５３℃まで冷却した
後、過酸化水素水和物結晶を種結晶として０．５ｇ添加
し、当該原料過酸化水素中に固相を少量析出せしめた。
さらに冷却を強化し、水溶液の温度が−５４．５℃にな
るまで冷却して固相の析出を行った。種結晶を添加して
から−５４．５℃まで冷却するまでの時間（固相の析出
時間）は５時間であった。続いて析出した固相を回収
し、この結晶をバスケット型の遠心分離器に入れ、一部
の結晶を融解させながら固相を液相から分離する操作を
行った。得られた固相を融解し、５５０ｇの４８．８重
量％の過酸化水素水溶液を得た。（以下、この操作を凍
結精製操作と言う。）Example 1 Hydrogen peroxide was added to a stainless steel container having an internal volume of 2 L in an amount of 5%.
2200 g of an aqueous solution of hydrogen peroxide containing 5% by weight was added as a raw material, and the aqueous solution was cooled to −53 ° C. with stirring, and then 0.5 g of hydrogen peroxide hydrate crystals was added as a seed crystal. A small amount of solid phase was deposited therein.
The cooling was further strengthened, and the solid phase was deposited by cooling until the temperature of the aqueous solution reached −54.5 ° C. The time from the addition of the seed crystal to the cooling to −54.5 ° C. (solid phase deposition time) was 5 hours. Subsequently, the precipitated solid phase was collected, the crystals were placed in a basket-type centrifuge, and the solid phase was separated from the liquid phase while melting some crystals. The obtained solid phase was melted to obtain 550 g of a 48.8 wt% hydrogen peroxide aqueous solution. (Hereinafter, this operation is referred to as a freeze purification operation.)
【００２０】得られた過酸化水素水溶液を過酸化水素濃
度３１重量％に希釈した後、１０００ｍｌ／ｈｒで、カ
チオン交換樹脂充填カラム、アニオン交換樹脂充填カラ
ム、カチオン交換樹脂とアニオン交換樹脂の混合物充填
カラムの順に通液した。各充填カラムは、それぞれ内径
２０ｍｍφのフッ素樹脂製カラム管に２０ｍｌずつイオ
ン交換樹脂を充填して作製した。カチオン交換樹脂充填
カラムには三菱化成工業（株）製、商品名ダイアイオン
ＰＫ２２８ＬＨを、アニオン交換樹脂充填カラムには三
菱化成工業（株）製、商品名ダイアイオンＰＡ３１８Ｈ
ＣＯ３を、混合物充填カラムにはカチオン交換樹脂（ダ
イアイオンＰＫ２２８ＬＨ）とアニオン交換樹脂（ダイ
アイオンＰＡ３１８ＨＣＯ３）の体積比１：１の混合物
を使用した。The obtained aqueous hydrogen peroxide solution was diluted to a hydrogen peroxide concentration of 31% by weight and then, at 1000 ml / hr, a cation exchange resin packed column, an anion exchange resin packed column, and a mixture of a cation exchange resin and an anion exchange resin were packed. The solution was passed through the column in this order. Each packed column was prepared by packing 20 ml of an ion exchange resin into a fluororesin column tube having an inner diameter of 20 mmφ. Cation exchange resin packed column is Mitsubishi Kasei Kogyo Co., Ltd., trade name Diaion PK228LH, anion exchange resin packed column is Mitsubishi Kasei Co., Ltd. trade name, Diaion PA318H.
CO3 was used in the mixture packed column using a mixture of a cation exchange resin (Diaion PK228LH) and an anion exchange resin (Diaion PA318HCO3) in a volume ratio of 1: 1.
【００２１】精製後の不純物含有量は第１表に示した如
くであり、カチオン不純物０．５ｐｐｂ以下、アニオン
不純物１０ｐｐｂ以下、有機不純物は全有機炭素量とし
て１ｍｇ／Ｌ以下が達成された。The content of impurities after purification was as shown in Table 1. Cationic impurities were 0.5 ppb or less, anionic impurities were 10 ppb or less, and organic impurities were 1 mg / L or less as the total organic carbon content.
【００２２】対照例１ 容器からの金属の溶出がないことを確認するためにブラ
ンク試験を行った。すなわち、実施例１で使用したステ
ンレス製容器の中に原料として５５重量％過酸化水素水
溶液２２００ｇを入れ、−５５℃で２４時間攪拌した
後、常温に戻し、過酸化水素水溶液中の不純物を分析し
た。操作後の過酸化水素水溶液は、操作前の原料過酸化
水素水溶液と比較して、含有される不純物は増加も減少
もしていなかった。Control Example 1 A blank test was conducted to confirm that no metal was eluted from the container. That is, 2200 g of a 55 wt% hydrogen peroxide aqueous solution was placed as a raw material in the stainless steel container used in Example 1, stirred at −55 ° C. for 24 hours, then returned to room temperature, and analyzed for impurities in the hydrogen peroxide aqueous solution. did. In the hydrogen peroxide aqueous solution after the operation, the contained impurities were neither increased nor decreased as compared with the raw material hydrogen peroxide aqueous solution before the operation.
【００２３】比較例１ 原料過酸化水素水溶液を過酸化水素濃度３１重量％に希
釈した後、実施例１と同様にして、１０００ｍｌ／ｈｒ
で、カチオン交換樹脂充填カラム、アニオン交換樹脂充
填カラム、カチオン交換樹脂とアニオン交換樹脂の混合
物充填カラムの順に通液した。得られた過酸化水素水溶
液を過酸化水素濃度５５重量％に濃縮した後、実施例１
と同様にして、凍結精製操作を行った。得られた過酸化
水素水溶液中の不純物の分析結果を第１表に示す。実施
例１で得られた過酸化水素水溶液に比べて含有する不純
物レベルが高かった。Comparative Example 1 A raw material hydrogen peroxide solution was diluted to a hydrogen peroxide concentration of 31% by weight, and then 1000 ml / hr was prepared in the same manner as in Example 1.
Then, a cation exchange resin packed column, an anion exchange resin packed column, and a mixture packed column of a cation exchange resin and an anion exchange resin were passed in this order. After concentrating the obtained hydrogen peroxide aqueous solution to a hydrogen peroxide concentration of 55% by weight, Example 1
A freeze purification operation was performed in the same manner as in. Table 1 shows the analysis results of impurities in the obtained hydrogen peroxide aqueous solution. The level of impurities contained was higher than that of the hydrogen peroxide aqueous solution obtained in Example 1.
【００２４】[0024]
【表１】 第１表 過酸化水素水溶液中の不純物
（単位：ppb) Ａｌ Ｆｅ Ｎｉ Ｃｒ Ｃｌ ＳＯ4 ＴＯＣ(*) 原料 79 6 0.6 1.5 8 8 10 実施例１ 0.06 0.19 0.04 0.03 3 2 0.6 比較例１ 0.20 0.28 0.12 0.17 3 5 0.6 (*) ＴＯＣの単位はmg/L。[Table 1] Table 1 Impurities in hydrogen peroxide solution (unit: ppb) Al Fe Ni Cr Cl SO 4 TOC (*) Raw material 79 6 0.6 1.5 8 8 10 Example 1 0.06 0.19 0.04 0.03 3 2 0.6 Comparative example 1 0.20 0.28 0.12 0.17 3 5 0.6 (*) TOC unit is mg / L.
【００２５】[0025]
【発明の効果】本発明によれば、無機不純物及び有機不
純物を含む不純過酸化水素水溶液を精製し、これらの含
有量がいずれも極めて低いレベルにまで低下した、高純
度の過酸化水素水溶液を工業的に安全に得る方法が提供
される。According to the present invention, an impure hydrogen peroxide aqueous solution containing an inorganic impurity and an organic impurity is purified, and a highly pure hydrogen peroxide aqueous solution in which the content of each of them is reduced to an extremely low level is obtained. An industrially safe method is provided.
Claims (3)
５．２重量％以上の濃度の過酸化水素水溶液を原料とし
てこれを冷却して固相を析出させ、かかる固相を回収
し、融解した後、さらに、カチオン交換樹脂層、アニオ
ン交換樹脂層並びにカチオン交換樹脂及びアニオン交換
樹脂の混合層からなる群から選ばれた少なくとも２種の
互いに異なる層に通液せしめることを特徴とする、過酸
化水素水溶液の精製法。1. When purifying an aqueous hydrogen peroxide solution, 4
A hydrogen peroxide aqueous solution having a concentration of 5.2% by weight or more is used as a raw material, which is cooled to precipitate a solid phase, the solid phase is recovered and melted, and then a cation exchange resin layer, an anion exchange resin layer and A method for purifying an aqueous hydrogen peroxide solution, which comprises passing the solution through at least two different layers selected from the group consisting of a mixed layer of a cation exchange resin and an anion exchange resin.
量％以上６０重量％未満の濃度を有する過酸化水素水溶
液を使用する、請求項１記載の過酸化水素水溶液の精製
法。2. The method for purifying an aqueous hydrogen peroxide solution according to claim 1, wherein an aqueous hydrogen peroxide solution having a concentration of 45.2% by weight or more and less than 60% by weight is used as the starting hydrogen peroxide solution.
求項１記載の過酸化水素水溶液の精製法。3. The method for purifying an aqueous hydrogen peroxide solution according to claim 1, wherein the solid phase is deposited for 3 to 16 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4853595A JPH08245204A (en) | 1995-03-08 | 1995-03-08 | Refining method of hydrogen peroxide aqueous solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4853595A JPH08245204A (en) | 1995-03-08 | 1995-03-08 | Refining method of hydrogen peroxide aqueous solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08245204A true JPH08245204A (en) | 1996-09-24 |
Family
ID=12806065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4853595A Pending JPH08245204A (en) | 1995-03-08 | 1995-03-08 | Refining method of hydrogen peroxide aqueous solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08245204A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0846654A1 (en) * | 1996-12-05 | 1998-06-10 | Startec Ventures, Inc. | On-site manufacture of ultra-high-purity hydrogen peroxide |
| WO2018021038A1 (en) * | 2016-07-29 | 2018-02-01 | 富士フイルム株式会社 | Treatment liquid and method for washing substrate |
| CN109775665A (en) * | 2019-03-30 | 2019-05-21 | 王晓华 | Hydrogen peroxide purifies production system |
-
1995
- 1995-03-08 JP JP4853595A patent/JPH08245204A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0846654A1 (en) * | 1996-12-05 | 1998-06-10 | Startec Ventures, Inc. | On-site manufacture of ultra-high-purity hydrogen peroxide |
| WO2018021038A1 (en) * | 2016-07-29 | 2018-02-01 | 富士フイルム株式会社 | Treatment liquid and method for washing substrate |
| KR20190015412A (en) * | 2016-07-29 | 2019-02-13 | 후지필름 가부시키가이샤 | Process liquid and substrate cleaning method |
| JPWO2018021038A1 (en) * | 2016-07-29 | 2019-05-30 | 富士フイルム株式会社 | Processing solution and substrate cleaning method |
| US10626356B2 (en) | 2016-07-29 | 2020-04-21 | Fujifilm Corporation | Treatment liquid and method for washing substrate |
| TWI709644B (en) * | 2016-07-29 | 2020-11-11 | 日商富士軟片股份有限公司 | Treatment liquid and substrate cleaning method |
| CN109775665A (en) * | 2019-03-30 | 2019-05-21 | 王晓华 | Hydrogen peroxide purifies production system |
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