JPH04202001A - Production of disodium trihydrogen paraperiodate - Google Patents
Production of disodium trihydrogen paraperiodateInfo
- Publication number
- JPH04202001A JPH04202001A JP33002990A JP33002990A JPH04202001A JP H04202001 A JPH04202001 A JP H04202001A JP 33002990 A JP33002990 A JP 33002990A JP 33002990 A JP33002990 A JP 33002990A JP H04202001 A JPH04202001 A JP H04202001A
- Authority
- JP
- Japan
- Prior art keywords
- sodium
- chlorine
- iodate
- paraperiodate
- added
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 title description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000460 chlorine Substances 0.000 claims abstract description 25
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 25
- NALMPLUMOWIVJC-UHFFFAOYSA-N n,n,4-trimethylbenzeneamine oxide Chemical compound CC1=CC=C([N+](C)(C)[O-])C=C1 NALMPLUMOWIVJC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011697 sodium iodate Substances 0.000 claims abstract description 20
- 235000015281 sodium iodate Nutrition 0.000 claims abstract description 20
- 229940032753 sodium iodate Drugs 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 12
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims abstract description 5
- 235000019799 monosodium phosphate Nutrition 0.000 claims abstract description 5
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 5
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 5
- VUSLYGKUDDJMMC-UHFFFAOYSA-N 2-bromo-[1,3]thiazolo[5,4-b]pyridine Chemical compound C1=CN=C2SC(Br)=NC2=C1 VUSLYGKUDDJMMC-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 229910052740 iodine Inorganic materials 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- -1 alkali metal iodates Chemical class 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
パラ過ヨウ素酸ナトリウムはメタ過ヨウ素酸ナトリウム
の製造に用いられる。また、メタ過ヨウ素酸ナトリウム
は、アルデヒドでんぷんの製造等に用いられる有用な化
合物である。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] Sodium para-periodate is used in the production of sodium meta-periodate. In addition, sodium metaperiodate is a useful compound used in the production of aldehyde starch and the like.
本発明はパラ過ヨウ素酸三水素二ナトリウムの製造法に
関する。The present invention relates to a method for producing disodium paraperiodate trihydrogen.
ヨウ素酸ナトリウムをアルカリ条件下、塩素により酸化
し、パラ過ヨウ素酸ナトリウムを得る方法としてＩｎｏ
ｒｇａｎｉｃ ５ｙｎｔｈｅｓｉｓ Ｃｏ１１ｅｃｔｉ
ｖｅ Ｖｏｌ。Ino is a method for obtaining sodium para-periodate by oxidizing sodium iodate with chlorine under alkaline conditions.
rganic 5ynthesis Co11ecti
ve Vol.
Ｉ、 ｐ、１６８〜１７１（１９）がある。 この方法
では、所定の水酸化ナトリウム水溶液中にヨウ素酸ナト
リウムを懸濁又は溶解させ、煮沸条件で急速に塩素を流
入することによりパラ過ヨウ素酸ナトリウムを得ている
。I, p, 168-171 (19). In this method, sodium paraperiodate is obtained by suspending or dissolving sodium iodate in a predetermined aqueous sodium hydroxide solution and rapidly introducing chlorine under boiling conditions.
この条件で生成するパラ過ヨウ素酸ナトリウムは三ナト
リウム塩であり、この結晶は微細であるために、濾過操
作等による分離が困難である。Sodium paraperiodate produced under these conditions is a trisodium salt, and the crystals are so fine that they are difficult to separate by filtration or the like.
この方法では、操作性の良好なパラ過ヨウ素酸の二ナト
リウム塩を選択的に得ることができない。With this method, it is not possible to selectively obtain the disodium salt of para-periodic acid, which has good operability.
また、塩素による酸化雰囲気下、高温かつ強アルカリ条
件下でのヨウ素酸アルカリ金属塩の酸化反応では、通常
の耐食性材料を使用することができない。 そのため、
汎用な材料からなる多目的反応器で容易にパラ過ヨウ素
酸ナトリウムを製造することができない。Furthermore, ordinary corrosion-resistant materials cannot be used in the oxidation reaction of alkali metal iodates under chlorine-based oxidizing atmosphere at high temperatures and under strong alkaline conditions. Therefore,
Sodium para-periodate cannot be easily produced using a multi-purpose reactor made of general-purpose materials.
本発明は、ヨウ素酸ナトリウムを塩素により酸化し、パ
ラ過ヨウ素酸ナトリウムを得る方法において、穏和な反
応条件下で、かつ、パラ過ヨウ素酸三水素二ナトリウム
を選択的に製造することを目的とする。The purpose of the present invention is to selectively produce disodium para-periodate under mild reaction conditions in a method for obtaining sodium para-periodate by oxidizing sodium iodate with chlorine. do.
本発明者らは、これらの問題点を解決するために鋭意検
討した結果、塩素酸化する際に、予め炭酸ナトリウム等
を添加した後に、水酸化ナトリウムを連続添加し、ＰＨ
を７〜１０に調製することが有効であることを見出し、
本発明を完成するに至った。As a result of intensive studies to solve these problems, the inventors of the present invention discovered that when performing chlorine oxidation, after adding sodium carbonate etc. in advance, sodium hydroxide was continuously added, and the PH
It has been found that it is effective to adjust the number to 7 to 10,
The present invention has now been completed.
すなわち、ヨウ素酸ナトリウムを塩素により酸化してパ
ラ過ヨウ素酸ナトリウムを得る方法において、予め、炭
酸水素ナトリウム、炭酸ナトリウム、リン酸二水素ナト
リウム、リン酸水素二ナトリウムのうち選ばれた１種類
以上の化合物を添加した後に、水酸化ナトリウムを連続
的に添加し、塩素による酸化時のｐＨを７〜１０の間に
調製することを特徴とするパラ過ヨウ素酸ナトリウムの
製造方法である。That is, in the method of obtaining sodium paraperiodate by oxidizing sodium iodate with chlorine, at least one selected from sodium bicarbonate, sodium carbonate, sodium dihydrogen phosphate, and disodium hydrogen phosphate is used in advance. This is a method for producing sodium para-periodate, which is characterized in that after adding the compound, sodium hydroxide is continuously added to adjust the pH during oxidation with chlorine to between 7 and 10.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず、原料のヨウ素酸ナトリウムは、ヨウ素を塩素酸ナ
トリウム水溶液中で酸化することにより得ることができ
るということがＩｎｏｒｇａｎｉｃ ５ｙｎｔｈ−ｅｓ
ｉｓ Ｃｏ１１ｅｃｔｉｖｅ Ｖｏｌ、Ｉ、 ｐ、１６
８−１７Ｈ１９）に記載しである。First, it is known that the raw material sodium iodate can be obtained by oxidizing iodine in an aqueous sodium chlorate solution.
is Colactive Vol, I, p, 16
8-17H19).
本発明では、これを改良し、具体的には以下のように調
製する。In the present invention, this is improved and specifically prepared as follows.
塩素酸ナトリウムの量は、ヨウ素分子１モルに対・して
、１．８〜２．４モル用いることが好ましく、２．４モ
ルを越えても、反応の効率に差がなく、経済的ではない
。The amount of sodium chlorate used is preferably 1.8 to 2.4 moles per mole of iodine molecules. Even if it exceeds 2.4 moles, there is no difference in reaction efficiency and it is not economical. do not have.
ヨウ素の酸化を行うためには、酸を添加する必要がある
。 酸としては、塩酸、硫酸、硝酸、リン酸、過塩素酸
等を用いることができる。In order to oxidize iodine, it is necessary to add acid. As the acid, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, etc. can be used.
酸の添加量は、ヨウ素分子１モルに対して、通常０．１
〜１０モル％、好ましくは、０．５〜５モル％である。The amount of acid added is usually 0.1 per mole of iodine molecules.
-10 mol%, preferably 0.5-5 mol%.
反応温度は、５５°Ｃ以上が望ましく、反応時間は反応
温度により異なるが、１．０〜３．０時間である。The reaction temperature is preferably 55°C or higher, and the reaction time varies depending on the reaction temperature, but is 1.0 to 3.0 hours.
得られるヨウ素酸ナトリウム水溶液の濃度を１０〜５０
重量％になるように調製する。The concentration of the obtained sodium iodate aqueous solution is 10 to 50.
Adjust to % by weight.
前記ヨウ素酸ナトリウム水溶液、又は、別に、精製した
ヨウ素酸ナトリウムを上記濃度になるように水に溶解さ
せた水溶液を用いて、パラ過ヨウ素酸ナトリウムを製造
する。Sodium para-periodate is produced using the aqueous sodium iodate solution or, separately, an aqueous solution in which purified sodium iodate is dissolved in water to the above concentration.
ヨウ素酸ナトリウム水溶液のｐＨが低すぎる場合は、所
定のｐＨになるように塩基で調製を行う。If the pH of the sodium iodate aqueous solution is too low, adjust it to a predetermined pH using a base.
所定のｐＨとは、ヨウ素酸ナトリウムを塩素で酸化する
際に適するｐＨのことであり、７〜１０の間である。The predetermined pH is a pH suitable for oxidizing sodium iodate with chlorine, and is between 7 and 10.
ｐＨの調製に用いる塩基は、炭酸水素ナトリウム、炭酸
ナトリウム等の炭酸塩、リン酸二水素ナトリウム、リン
酸水素二ナトリウム等のリン酸塩のうち選ばれた１種類
以上の塩、及び水酸化ナトリウムである。 これらの形
状は、固体又は水）容液である。 このｐＨ調製の時期
は、昇温しで塩素による酸化反応を開始する前までに行
えばよい。The base used for pH adjustment is one or more salts selected from carbonates such as sodium hydrogen carbonate and sodium carbonate, phosphates such as sodium dihydrogen phosphate and disodium hydrogen phosphate, and sodium hydroxide. It is. These forms are solid or water-based. This pH adjustment may be carried out before the temperature is raised and the oxidation reaction by chlorine is started.
塩素による酸化反応は、ＰＨが７〜１０を保持するよう
に、水酸化ナトリウムと塩素を連続的に添加しながら行
う。The oxidation reaction with chlorine is performed while continuously adding sodium hydroxide and chlorine so that the pH is maintained at 7 to 10.
また、このｐＨ範囲を保持し易くするために、炭酸水素
ナトリウム、炭酸ナトリウム等の炭酸塩やリン酸二水素
ナトリウム、リン酸水素二ナトリウム等のリン酸塩のう
ち、１種類以上の塩を、予め添加する。In addition, in order to easily maintain this pH range, one or more salts among carbonates such as sodium hydrogen carbonate and sodium carbonate, and phosphates such as sodium dihydrogen phosphate and disodium hydrogen phosphate, Add in advance.
これら塩の添加量は、ヨウ素酸ナトリウム１モルに対し
て、０．２〜２．０モルが望ましい。The amount of these salts added is preferably 0.2 to 2.0 mol per 1 mol of sodium iodate.
酸化反応の温度は、５０°Ｃ以上、好ましくは、７０°
Ｃ以上である。 水溶液中での反応であるため、反応温
度は、水溶液の沸点までで行うことが望ましいが、加圧
することによって、それ以上の温度でも反応することが
できる。The temperature of the oxidation reaction is 50°C or higher, preferably 70°C.
C or higher. Since the reaction is carried out in an aqueous solution, the reaction temperature is preferably up to the boiling point of the aqueous solution, but the reaction can be carried out at a higher temperature by applying pressure.
連続的に添加する水酸化ナトリウムは、水溶液で用いる
ことが望ましい。 水酸化ナトリウム水溶液の濃度は、
低すぎると生産性が低下するため２０重量％以上が望ま
しい。もちろん、操作性に問題なければ、固体の状態で
も添加することができる。It is desirable to use the continuously added sodium hydroxide in the form of an aqueous solution. The concentration of sodium hydroxide aqueous solution is
If it is too low, productivity will decrease, so 20% by weight or more is desirable. Of course, it can be added in solid form if there is no problem with operability.
添加する水酸化ナトリウムの量は、前記塩類の添加量に
よっても異なるが、ヨウ素酸ナトリウム１モルに対して
３．０〜６．０モル程度が好ましい。The amount of sodium hydroxide added varies depending on the amount of the salts added, but is preferably about 3.0 to 6.0 mol per 1 mol of sodium iodate.
この量が３．０モル未満では、ヨウ素酸ナトリウムの転
化率が低下し、パラ過ヨウ素酸ナトリウムの収率が低゛
下し、好ましくない。 また、６．０モルを越えて使用
しても、収率の向上はない。If this amount is less than 3.0 moles, the conversion rate of sodium iodate will decrease and the yield of sodium para-periodate will decrease, which is not preferable. Moreover, even if more than 6.0 mol is used, the yield will not improve.
塩素量は、添加する塩基の量によって異なるため一概に
は言えない。 塩素の導入は、塩基の添加を終了した時
点で終了する。The amount of chlorine cannot be determined unconditionally because it varies depending on the amount of base added. The introduction of chlorine ends when the addition of the base ends.
・塩素による酸化反応終了後、析出するパラ過ヨウ素酸
ナトリウムを濾過することにより結晶を得ることができ
る。- After completion of the oxidation reaction with chlorine, crystals can be obtained by filtering the precipitated sodium paraperiodate.
本発明における方法では、パラ過ヨウ素酸ナトリウムは
、選択的にニナトリウム塩として得られる。In the process according to the invention, sodium paraperiodate is optionally obtained as the disodium salt.
このニナトリウム塩は、従来技術で得られる三ナトリウ
ム塩と比較して、結晶性がよく、操作性が良好である。This disodium salt has better crystallinity and better operability than the trisodium salt obtained by conventional techniques.
以下、実施例により本発明の詳細な説明する。 Hereinafter, the present invention will be explained in detail with reference to Examples.
以下において、「％」は、特記する以外はモル基準であ
る。In the following, "%" is on a molar basis unless otherwise specified.
なお、パラ過ヨウ素酸ナトリウムの定量は、ヨウ素滴定
によった。Note that sodium paraperiodate was determined by iodometric titration.
実施例１
ヨウ素酸ナトリウム１５．０ｇ （０，１０モル）を水
１１２．５ ｇに懸濁させた。炭酸水素すトリウム８．
４ｇ （０，１０モル）を添加し、９０°Ｃに昇温した
。昇温後、３５Ｎｆｔ％水酸化ナトリウム水溶液４５．
７ｇ・（０，４０モル）を３０分間で添加しながら、ｐ
Ｈ８，０を保持するように塩素を導入した。水酸化ナ
トリウム水溶液の添加終了と同時に塩素の添加を止め、
３０°Ｃまで冷却した。Example 1 15.0 g (0.10 mol) of sodium iodate were suspended in 112.5 g of water. Thorium hydrogen carbonate8.
4 g (0.10 mol) was added and the temperature was raised to 90°C. After raising the temperature, add 35Nft% sodium hydroxide aqueous solution 45.
While adding 7 g (0.40 mol) in 30 minutes, p.
Chlorine was introduced to maintain H8.0. At the same time as the addition of the sodium hydroxide aqueous solution is completed, the addition of chlorine is stopped.
Cooled to 30°C.
析出する結晶を濾過し、水により充分に洗浄し、乾燥し
、パラ過ヨウ素酸ナトリウムの結晶２７．１ｇを得た。The precipitated crystals were filtered, thoroughly washed with water, and dried to obtain 27.1 g of sodium paraperiodate crystals.
この結晶の純度は９９．０％であり、パラ過ヨウ素酸三
水素二ナトリウムの収率は、９９．０％であった。The purity of this crystal was 99.0%, and the yield of disodium paraperiodate trihydrogen was 99.0%.
実施例２
実施例１において、炭酸水素ナトリウム８．４ｇ（０，
１０モル）を炭酸ナトリウム１０．６ｇ （０，１０モ
ル）及び、塩素導入時のｐＨを９．０に変えた以外、全
く同様に操作して、パラ過ヨウ素酸ナトリウムの結晶２
７．０ｇを得た。Example 2 In Example 1, 8.4 g (0,
Crystals of sodium para-periodate were prepared in exactly the same manner except that 10.6 g (0.10 mol) of sodium carbonate and the pH at the time of chlorine introduction were changed to 9.0.
7.0g was obtained.
この結晶の純度は、９９．２％であり、パラ過ヨウ素酸
三水素二ナトリウムの収率は、９８．５％であった。The purity of this crystal was 99.2%, and the yield of disodium paraperiodate trihydrogen was 98.5%.
実施例３
実施例１において、炭酸水素ナトリウム８．４ｇ（０，
１０モル）をリン酸水素二ナトリウム１４．２ｇ・（０
，１０モル）に代えた以外、全く同様に操作して、パラ
過ヨウ素酸ナトリウムの結晶２６．９ｇを得た。Example 3 In Example 1, 8.4 g of sodium hydrogen carbonate (0,
10 moles) and 14.2 g of disodium hydrogen phosphate (0
, 10 mol) was carried out in exactly the same manner to obtain 26.9 g of crystals of sodium para-periodate.
この結晶の純度は、９９．０％であり、パラ過ヨウ素酸
三水素二ナトリウムの収率は、９７．９％であった。The purity of this crystal was 99.0%, and the yield of disodium paraperiodate trihydrogen was 97.9%.
比較例１
実施例１ムこおいて、３５重景％水酸化ナトリウム水溶
液の量を増して塩素導入時のｐＨを１３．０に変えた以
外、全く同様に操作して、パラ過ヨウ素酸ナトリウムの
結晶２９．２ｇを得た。Comparative Example 1 Sodium para-periodate was prepared in exactly the same manner as in Example 1 except that the amount of the 35% sodium hydroxide aqueous solution was increased and the pH at the time of chlorine introduction was changed to 13.0. 29.2 g of crystals were obtained.
この結晶の純度は、９０．３％であり、パラ過ヨウ素酸
三水素二ナトリウムの収率は、９７．０％であった。The purity of this crystal was 90.3%, and the yield of disodium paraperiodate trihydrogen was 97.0%.
比較例２
実施例３において、塩素導入時のｐＨを６．０とした以
外、全く同様に操作して、パラ過ヨウ素酸ナトリウムの
結晶１２．４ｇを得た。Comparative Example 2 The same procedure as in Example 3 was carried out except that the pH at the time of chlorine introduction was changed to 6.0 to obtain 12.4 g of crystals of sodium para-periodate.
この結晶の純度は、９９．０％であり、パラ過ヨウ素酸
三水素二ナトリウムの収率は、４５．１％であった。The purity of this crystal was 99.0%, and the yield of disodium paraperiodate trihydrogen was 45.1%.
本発明によれば、従来技術では不可能であった選択的に
パラ過ヨウ素酸三水素二ナトリウムを得ることができる
。 そのため、結晶の操作性も良好である。According to the present invention, it is possible to selectively obtain disodium paraperiodate trihydrogen, which was not possible with the prior art. Therefore, the operability of the crystal is also good.
また、この際の反応条件が穏和であるために、グラスラ
イニングのような汎用材料からなる多目的反応器で、容
易にパラ過ヨウ素酸ナトリウムを製造することができる
。Moreover, since the reaction conditions at this time are mild, sodium para-periodate can be easily produced in a multipurpose reactor made of a general-purpose material such as glass lining.
Claims (1)
過ヨウ素酸ナトリウムを得る方法において、予め、炭酸
水素ナトリウム、炭酸ナトリウム、リン酸二水素ナトリ
ウム、リン酸水素二ナトリウムのうち選ばれた１種類以
上の化合物を添加した後に、水酸化ナトリウムを連続的
に添加し、塩素による酸化時のｐＨを７〜１０の間に調
製することを特徴とするパラ過ヨウ素酸ナトリウムの製
造方法。(1) In the method of obtaining sodium paraperiodate by oxidizing sodium iodate with chlorine, one type selected in advance from sodium hydrogen carbonate, sodium carbonate, sodium dihydrogen phosphate, and disodium hydrogen phosphate is used. A method for producing sodium paraperiodate, which comprises continuously adding sodium hydroxide after adding the above compound to adjust the pH during oxidation with chlorine to between 7 and 10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33002990A JP2912444B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing disodium trihydrogen periodate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33002990A JP2912444B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing disodium trihydrogen periodate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04202001A true JPH04202001A (en) | 1992-07-22 |
| JP2912444B2 JP2912444B2 (en) | 1999-06-28 |
Family
ID=18227983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33002990A Expired - Fee Related JP2912444B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing disodium trihydrogen periodate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2912444B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1007395C2 (en) * | 1997-10-30 | 1999-05-04 | Dsm Nv | Process for the preparation of periodates. |
| WO2004083117A1 (en) * | 2003-03-19 | 2004-09-30 | Sumitomo Chemical Company, Limited | Method for preparing disodium paraperiodate |
| JP2004300023A (en) * | 2003-03-19 | 2004-10-28 | Sumitomo Chem Co Ltd | Method for producing disodium para-periodate |
-
1990
- 1990-11-30 JP JP33002990A patent/JP2912444B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1007395C2 (en) * | 1997-10-30 | 1999-05-04 | Dsm Nv | Process for the preparation of periodates. |
| EP0913358A1 (en) * | 1997-10-30 | 1999-05-06 | Dsm N.V. | Process for the preparation of periodates |
| WO2004083117A1 (en) * | 2003-03-19 | 2004-09-30 | Sumitomo Chemical Company, Limited | Method for preparing disodium paraperiodate |
| JP2004300023A (en) * | 2003-03-19 | 2004-10-28 | Sumitomo Chem Co Ltd | Method for producing disodium para-periodate |
| US7179439B2 (en) | 2003-03-19 | 2007-02-20 | Sumitomo Chemical Company, Limited | Method for preparing disodium paraperiodate |
| CN100404410C (en) * | 2003-03-19 | 2008-07-23 | 住友化学株式会社 | Method for preparing disodium paraperiodate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2912444B2 (en) | 1999-06-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPS58114740A (en) | Recovery and reuse of cobalt and/or manganese catalytic component | |
| JPH04202001A (en) | Production of disodium trihydrogen paraperiodate | |
| JP2912445B2 (en) | Method for producing alkali metal periodate | |
| KR20060129524A (en) | METHOD FOR PROCESSING beta;-SULPHATOETHYLSULPHONYLANILINE-2-SULPHONIC ACID | |
| CN110817883A (en) | Process for producing potassium fluosilicate by using byproduct calcium fluoride | |
| JP4079991B2 (en) | Method for producing cesium salt from cesium aluminum alum | |
| JP2912446B2 (en) | Method for producing sodium metaperiodate | |
| JP2870183B2 (en) | Process for producing 1,3-phenylenedioxydiacetic acid | |
| JPS643199B2 (en) | ||
| JP2917498B2 (en) | Process for producing 1,3-phenylenedioxydiacetic acid | |
| JP3545658B2 (en) | Method for producing iridium nitrate solution | |
| US4203955A (en) | Process of preparing calcium hydrogen phosphate anhydride suitable as material for phosphors | |
| JP3326867B2 (en) | Method for producing metal salt of iminodisuccinic acid | |
| JP2006248857A (en) | METHOD OF MANUFACTURING beta-MnOOH | |
| JPH06115904A (en) | Production of potassium periodate | |
| RU2102324C1 (en) | Method for producing titanium dioxide | |
| JPH0665244A (en) | Purification of riboflavin | |
| JP3444876B2 (en) | Method for producing basic magnesium hypochlorite | |
| JPH04273844A (en) | Preparation of 2,2'-oxydisuccinic acid salt | |
| JP2005067944A (en) | Method for producing iodic acid | |
| SU406821A1 (en) | METHOD OF OBTAINING TETRACENE | |
| JPH06329606A (en) | Production of iminodisuccinic acid metal salt | |
| EP0861841B1 (en) | Process for producing 2-amino-6-iodopurine | |
| JP4596833B2 (en) | Method for producing periodate | |
| JPH0788336B2 (en) | Process for producing 5-amino-2,4,6-triiodoisophthalic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |