JPH04202002A - Production of alkali metal periodate - Google Patents
Production of alkali metal periodateInfo
- Publication number
- JPH04202002A JPH04202002A JP33003090A JP33003090A JPH04202002A JP H04202002 A JPH04202002 A JP H04202002A JP 33003090 A JP33003090 A JP 33003090A JP 33003090 A JP33003090 A JP 33003090A JP H04202002 A JPH04202002 A JP H04202002A
- Authority
- JP
- Japan
- Prior art keywords
- alkali metal
- chlorine
- iodate
- periodate
- alkali
- 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
- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 32
- -1 alkali metal periodate Chemical class 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000460 chlorine Substances 0.000 claims abstract description 27
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 27
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 9
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical class OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 8
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 18
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- NALMPLUMOWIVJC-UHFFFAOYSA-N n,n,4-trimethylbenzeneamine oxide Chemical compound CC1=CC=C([N+](C)(C)[O-])C=C1 NALMPLUMOWIVJC-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011697 sodium iodate Substances 0.000 abstract description 5
- 235000015281 sodium iodate Nutrition 0.000 abstract description 5
- 229940032753 sodium iodate Drugs 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000000725 suspension Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229910052740 iodine Inorganic materials 0.000 description 5
- MLIWQXBKMZNZNF-KUHOPJCQSA-N (2e)-2,6-bis[(4-azidophenyl)methylidene]-4-methylcyclohexan-1-one Chemical compound O=C1\C(=C\C=2C=CC(=CC=2)N=[N+]=[N-])CC(C)CC1=CC1=CC=C(N=[N+]=[N-])C=C1 MLIWQXBKMZNZNF-KUHOPJCQSA-N 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 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 description 3
- 239000002253 acid Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M chlorate Inorganic materials [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 3
- 239000001230 potassium iodate Substances 0.000 description 3
- 235000006666 potassium iodate Nutrition 0.000 description 3
- 229940093930 potassium iodate Drugs 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 241000220317 Rosa Species 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000002244 precipitate Substances 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
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical class [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
・過ヨウ素酸アルカリ金属塩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] - Periodate alkali metal salt is a useful compound used in the production of aldehyde starch, etc.
本発明は、過ヨウ素酸アルカリ金属塩の製造法に関する
。The present invention relates to a method for producing an alkali metal periodate salt.
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、
Ｉｎｏｒｇａｎｉｃ ５ｙｎｔｈｅｓｉｓ Ｃｏ１１ｅ
ｃｔｉｖｅＶｏ１．Ｉ 、 ｐ、１６８〜１７１（１９
）がある。As a method for obtaining sodium para-periodate by oxidizing sodium iodate with chlorine under alkaline conditions,
Inorganic 5ynthesis Co11e
activeVol1. I, p, 168-171 (19
).
また、過ヨウ素酸カリウムの製造法として、ヨウ素酸カ
リウムを水酸化カリウム水溶液中で塩素により酸化する
方法■が日本化学会編、新実験化学講座、８巻、 ｐ、
５２５（１９７５）、丸首に示されている。In addition, as a method for producing potassium periodate, a method ■ in which potassium iodate is oxidized with chlorine in an aqueous potassium hydroxide solution is edited by the Chemical Society of Japan, New Experimental Chemistry Course, vol. 8, p.
525 (1975), shown in the round neck.
また、酸素によりヨウ素酸ナトリウム又はヨウ素酸カリ
ウムを酸化し、過ヨウ素酸塩を製造する方法■が、米国
特許第４１７６１６７号に示されている。Further, US Pat. No. 4,176,167 discloses a method (2) for producing periodate by oxidizing sodium iodate or potassium iodate with oxygen.
また、過ヨウ素酸塩を電解酸化により製造する方法■が
、特開昭５７−１９４２８号公報に示されている。Further, method (2) for producing periodate by electrolytic oxidation is disclosed in JP-A-57-19428.
まず、酸素酸化による上記■の方法では、選択率よく過
ヨウ素酸塩を得るためには、３００°Ｃ付近の温度及び
酸素加圧の条件で反応させなければならない。First, in method (2) using oxygen oxidation, in order to obtain periodate with good selectivity, the reaction must be carried out at a temperature around 300° C. and under oxygen pressurization conditions.
また、電解酸化による上記■の方法では、電極等に特殊
な材料を使用する必要がある。Further, in the above method (1) using electrolytic oxidation, it is necessary to use special materials for electrodes and the like.
これら■及び■の方法では、装置的に特殊なものが必要
であるため汎用性のある反応器を用いることができない
。These methods (1) and (2) require special equipment and cannot use a versatile reactor.
次に、塩゛素酸化による上記■及び■の方法では、所定
の水酸化アルカリ金属水溶液中にヨウ素酸アルカリ金属
を懸濁又は溶解させ、煮沸条件で急速に塩素を流入する
ことにより過ヨウ素酸アルカリ金属塩を得ている。Next, in the methods (2) and (2) above using chlorine oxidation, an alkali metal iodate is suspended or dissolved in a predetermined aqueous alkali metal hydroxide solution, and chlorine is rapidly introduced under boiling conditions to oxidize periodate. Alkali metal salts are obtained.
塩素による酸化雰囲気下で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では、条件的に過酷で
ある。 そのため、通常の耐食性材料からなる汎用な反
応器を用いて、過ヨウ素酸アルカリ金属塩を製造するこ
とができない。Oxidation of alkali metal iodate under oxidizing atmosphere with chlorine at high temperature and under strong alkaline conditions is harsh. Therefore, periodate alkali metal salts cannot be produced using general-purpose reactors made of ordinary corrosion-resistant materials.
本発明は、ヨウ素酸アルカリ金属塩を塩素により酸化し
、過ヨウ素酸アルカリ金属塩を得る方法において、穏和
な条件下で製造することを目的とする。The object of the present invention is to produce an alkali metal periodate under mild conditions in a method of obtaining an alkali metal salt of periodate by oxidizing an alkali metal salt of iodate with chlorine.
本発明者らは、上記問題を解決するために鋭意検討した
結果、塩素酸化する際に、アルカリを連続添加し、ｐＨ
を７〜１ｏ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 the above problems, the inventors of the present invention have found that when oxidizing chlorine, alkali is continuously added, and the pH
It was found that it is effective to adjust the temperature to 7 to 1o,
The present invention has now been completed.
すなわち、ヨウ素酸アルカリ金属塩を塩素により酸化し
て過ヨウ素酸アルカリ金属塩を得る方法において、塩素
による酸化時のＰＨを７〜１ｏの間に調製することを特
徴とする過ヨウ素酸アルカリ金属塩の製造方法である。That is, in a method of obtaining an alkali metal periodate by oxidizing an alkali metal salt of iodate with chlorine, the alkali metal salt of periodate is characterized in that the pH during oxidation with chlorine is adjusted to between 7 and 1o. This is a manufacturing method.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず、原料のヨウ素酸アルカリ金属は、ヨウ素を塩素酸
アルカリ金属水溶液中で酸化することにより得ることが
できる。 このことは、上記■の文献に記載されている
が、米発明では、これを改良し、具体的には以下のよう
に調整する。First, the raw material alkali metal iodate can be obtained by oxidizing iodine in an aqueous alkali metal chlorate solution. This is described in the above-mentioned document (2), but in the US invention, this is improved and specifically adjusted as follows.
ヨウ素を酸化する塩素酸アルカリ金属の種類は、目的物
となる過ヨウ素酸アルカリ金属の種類によ・って異なる
が、塩素酸ナトリウム、塩素酸カリウム等が代表的であ
る。The type of alkali metal chlorate that oxidizes iodine varies depending on the type of the target alkali metal periodate, but sodium chlorate, potassium chlorate, etc. are typical examples.
塩素酸アルカリ金属の量は、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 alkali metal chlorate is preferably 1.8 to 2.4 moles per mole of iodine molecules, and even if it exceeds 2.4 moles, there is no difference in reaction efficiency and it is not economical. .
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.
得られるヨウ素酸アルカリ金属塩水溶液の濃度は、１０
〜５０重量％になるように調製する。The concentration of the alkali metal iodate salt aqueous solution obtained is 10
Adjust the amount to 50% by weight.
前記ヨウ素酸アルカリ金属塩水溶液、又は、別に、精製
したヨウ素酸アルカリ金属塩の結晶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、過ヨウ素酸アルカ
リ金属塩を製造する。An alkali metal periodate is produced using the aqueous solution of the alkali metal iodate, or separately, an aqueous solution in which purified alkali metal iodate crystals are dissolved in water to the above concentration.
ヨウ素酸アルカリ金属塩水溶液のｐＨが低すぎる場合は
、所定のｐＨになるようにアルカリで調製する。 所定
のｐＨとは、ヨウ素酸アルカリ金属塩を塩素で酸化する
際に適するＰＨのことであり、７〜１０の間である。If the pH of the aqueous alkali metal iodate solution is too low, adjust it to a predetermined pH using an alkali. The predetermined pH is a pH suitable for oxidizing an alkali metal iodate with chlorine, and is between 7 and 10.
ｐＨｔＪＲ製する場合、用いるアルカリの種類は、目的
物となる過ヨウ素酸アルカリ金属塩により異なる。
目的物がパラ過ヨウ素酸ナトリウムの場合、用いるアル
カリは水酸化ナトリウム、炭酸ナトリウム、炭酸水素ナ
トリウム、リン酸水素二ナトリウム、リン酸ナトリウム
等テある。When producing pHtJR, the type of alkali used varies depending on the target alkali metal periodate salt.
When the target product is sodium paraperiodate, the alkali to be used includes sodium hydroxide, sodium carbonate, sodium hydrogen carbonate, disodium hydrogen phosphate, and sodium phosphate.
目的物が過ヨウ素酸カリウムの場合、それは水酸化カリ
ウム、炭酸カリウム、リン酸水素二カリウム等となる。When the target product is potassium periodate, it becomes potassium hydroxide, potassium carbonate, dipotassium hydrogen phosphate, etc.
これらのアルカリの形状は、固体又は水溶液である。
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 form of these alkalis is solid or aqueous solution.
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 with chlorine is 50'C or higher, preferably 70"C or higher. Since the reaction is in an aqueous solution, it is desirable to carry out the reaction temperature up to the boiling point of the aqueous solution. By applying pressure, it is possible to react even at higher temperatures.
所定の温度において、前記アルカリを連続的に添加する
ことによって塩素による酸化を行う。Oxidation with chlorine is carried out by continuously adding the alkali at a predetermined temperature.
連続的に添加するアルカリは、水溶液で用いることが望
ましい。 このアルカリ水溶液の濃度は、低すぎると生
産性が低下するため２０重景％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アルカリを用
いることができる。The alkali that is added continuously is preferably used in the form of an aqueous solution. The concentration of this alkaline aqueous solution is desirably 20% or more because productivity decreases if it is too low. Of course, if there is no problem with operability, alkali can also be used in a solid state.
添加するアルカリの量は、アルカリの種類及び調製する
ｐＨ値によっても異なるが、ヨウ素酸アルカリ金属塩１
モルに対して３．０〜７．０モル程度が好ましい。
この量が３．０モル未満では、ヨウ素酸アルカリ金属塩
の転化率が低下し、過ヨウ素酸アルカリ金属塩の収率が
低下する。 また、７．０モルを越えて使用しても収率
の向上はない。The amount of alkali to be added varies depending on the type of alkali and the pH value to be prepared, but iodate alkali metal salt 1
It is preferably about 3.0 to 7.0 moles.
If this amount is less than 3.0 mol, the conversion rate of the alkali metal iodate will decrease, and the yield of the alkali metal periodate will decrease. Furthermore, even if more than 7.0 mol is used, the yield will not improve.
上記量のアルカリと塩素を連続的に添加しながらｐＨを
７〜１０に８周製する。The pH was adjusted to 7 to 10 for 8 cycles while continuously adding the above amounts of alkali and chlorine.
塩素量は添加するアルカリ量によって異なる。The amount of chlorine varies depending on the amount of alkali added.
塩素の導入は、水酸化アルカリ金属の添加を終了・した
時点で終了する。The introduction of chlorine ends when the addition of alkali metal hydroxide is completed.
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.
実施例１
ヨウ素酸ナトリウム３０．０ｇ （０，２０モル）を水
１２０ｇに懸濁させた。この懸濁液を９０°Ｃに昇温し
た。昇温後、３５重量％水酸化ナトリウム水溶液９１．
４ｇ （０，８０モル）を１時間で添加しながら、ＰＨ
９，０になるように塩素を添加した。水酸化ナトリウム
水溶液の添加が終了した時点で、塩素の添加も中止し、
反応液を３０°Ｃまで冷却した。Example 1 30.0 g (0.20 mol) of sodium iodate was suspended in 120 g of water. This suspension was heated to 90°C. After raising the temperature, add 35% by weight aqueous sodium hydroxide solution 91.
While adding 4 g (0.80 mol) in 1 hour, the PH
Chlorine was added to give a concentration of 9.0. When the addition of the sodium hydroxide aqueous solution is completed, the addition of chlorine is also stopped.
The reaction solution was cooled to 30°C.
析出する結晶を濾過し、充分の水で洗浄し、乾燥し、５
３．７ｇの結晶を得た。The precipitated crystals are filtered, washed with sufficient water, dried, and
3.7 g of crystals were obtained.
この結晶はバラ過ヨウ素酸三水素二ナトリウムであり、
その収率は９９．０％であった。This crystal is disodium trihydrogen rose periodate,
The yield was 99.0%.
実施例２
実施例１において、塩素添加時のｐＨを１０．０とした
以外は、全く同様に操作して、バラ過ヨウ素酸三水素二
ナトリウムの結晶５３．７ｇを得た。Example 2 The same procedure as in Example 1 was repeated except that the pH at the time of chlorine addition was changed to 10.0 to obtain 53.7 g of crystals of disodium trihydrogen rose periodate.
その収率は９８．７％であった。The yield was 98.7%.
実施例３
実施例１において、連続添加するアルカリの種類を炭酸
ナトリウムとした以外、全く同様に操作して、パラ過ヨ
ウ素酸三水素二ナトリウムの結晶２６．４ｇを得た。
その収率は９７．０％であった。Example 3 The same procedure as in Example 1 was repeated except that sodium carbonate was used as the alkali to be continuously added, to obtain 26.4 g of crystals of disodium trihydrogen paraperiodate.
The yield was 97.0%.
実施例４
実施例１において、ヨウ素酸ナトリウム０．２０モルを
ヨウ素酸カリウム０．２０モル、及び水酸化ナトリウム
水溶液０．８０モルを水酸化カリウム０．８０モルに代
えた以外、同様に反応を行った。Example 4 The reaction was carried out in the same manner as in Example 1, except that 0.20 mol of sodium iodate was replaced with 0.20 mol of potassium iodate, and 0.80 mol of sodium hydroxide aqueous solution was replaced with 0.80 mol of potassium hydroxide. went.
反応終了後、硝酸で中和し、結晶を析出させ、３０°Ｃ
まで冷却し、濾過し、結晶を冷水で洗浄し、乾燥した。After the reaction is complete, neutralize with nitric acid, precipitate crystals, and heat at 30°C.
Cool to , filter, wash the crystals with cold water and dry.
その結果、過ヨウ素酸カリウムの結晶４５．５ｇを得た
。As a result, 45.5 g of potassium periodate crystals were obtained.
比較例１
実施例１において、塩素添加時のｐＨを１３．０とした
以外、全く同様に操作して、６４．０ｇの結晶を得た。Comparative Example 1 64.0 g of crystals were obtained in exactly the same manner as in Example 1, except that the pH at the time of chlorine addition was changed to 13.0.
これは、パラ過ヨウ素酸ナトリウムの二ナトリウム
塩と三ナトリウム塩の混合物であった。This was a mixture of disodium and trisodium salts of sodium paraperiodate.
比較例２
実施例４において、塩素添加時のｐＨを１３．０とした
以外、全く同様に操作して、過ヨウ素酸カリウムの結晶
４５．４ｇを得た。その収率は９８．７％であった。Comparative Example 2 45.4 g of potassium periodate crystals were obtained in exactly the same manner as in Example 4, except that the pH at the time of chlorine addition was changed to 13.0. The yield was 98.7%.
以上の実施例１〜４及び比較例１．２の反応液を用いて
、グラスライニングの材質試験を行った。A glass lining material test was conducted using the reaction solutions of Examples 1 to 4 and Comparative Example 1.2.
試験方法は、各反応条件と同様の条件の反応液中に、グ
ラスライニング試験片を浸漬させ、１０００時間後に、
腐食状況を観察した。The test method was to immerse a glass lining test piece in a reaction solution under the same conditions as each reaction condition, and after 1000 hours,
The corrosion situation was observed.
その結果を第１表に示した。The results are shown in Table 1.
本発明によれば、従来技術では不可能であった汎用性の
高いグラスライニング製の反応器において、容易に過ヨ
ウ素酸アルカリ金属塩を製造することができる。According to the present invention, periodate alkali metal salts can be easily produced in a highly versatile glass-lined reactor, which was not possible with the prior art.
第１表 ○ 腐食なし、△ わずかな腐食 × 腐食ありTable 1 ○ No corrosion, △ Slight corrosion × Corrosion
Claims (1)
過ヨウ素酸アルカリ金属塩を得る方法において、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
とする過ヨウ素酸アルカリ金属塩の製造方法。(1) A method for obtaining an alkali periodate salt by oxidizing an alkali metal salt of iodate with chlorine, the method comprising adjusting the pH during oxidation with chlorine between 7 and 10. Method for producing metal salts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33003090A JP2912445B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali metal periodate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33003090A JP2912445B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali metal periodate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04202002A true JPH04202002A (en) | 1992-07-22 |
| JP2912445B2 JP2912445B2 (en) | 1999-06-28 |
Family
ID=18227993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33003090A Expired - Fee Related JP2912445B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali metal periodate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2912445B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6017506A (en) * | 1997-10-30 | 2000-01-25 | Dsm N.V. | Process for the preparation of periodates |
| US6455022B1 (en) * | 1991-06-10 | 2002-09-24 | Elf Atochem S.A. | Purification of aqueous alkali metal chloride solutions by removal of ammonium/iodine values therefrom |
| JP2004300023A (en) * | 2003-03-19 | 2004-10-28 | Sumitomo Chem Co Ltd | Method for producing disodium para-periodate |
| JP2006016266A (en) * | 2004-07-02 | 2006-01-19 | Toho Earthtech Inc | Method of manufacturing periodate |
-
1990
- 1990-11-30 JP JP33003090A patent/JP2912445B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6455022B1 (en) * | 1991-06-10 | 2002-09-24 | Elf Atochem S.A. | Purification of aqueous alkali metal chloride solutions by removal of ammonium/iodine values therefrom |
| US6017506A (en) * | 1997-10-30 | 2000-01-25 | Dsm N.V. | Process for the preparation of periodates |
| JP2004300023A (en) * | 2003-03-19 | 2004-10-28 | Sumitomo Chem Co Ltd | Method for producing disodium para-periodate |
| JP2006016266A (en) * | 2004-07-02 | 2006-01-19 | Toho Earthtech Inc | Method of manufacturing periodate |
| JP4596833B2 (en) * | 2004-07-02 | 2010-12-15 | 株式会社 東邦アーステック | Method for producing periodate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2912445B2 (en) | 1999-06-28 |
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