JPH0572324B2 - - Google Patents
Info
- Publication number
- JPH0572324B2 JPH0572324B2 JP19009086A JP19009086A JPH0572324B2 JP H0572324 B2 JPH0572324 B2 JP H0572324B2 JP 19009086 A JP19009086 A JP 19009086A JP 19009086 A JP19009086 A JP 19009086A JP H0572324 B2 JPH0572324 B2 JP H0572324B2
- Authority
- JP
- Japan
- Prior art keywords
- potassium
- hydrofluoric acid
- phosphate
- producing
- fluorophosphate
- 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 - Fee Related
Links
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 31
- 239000011591 potassium Substances 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 5
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 claims description 5
- 235000019828 potassium polyphosphate Nutrition 0.000 claims description 5
- 150000008064 anhydrides Chemical class 0.000 claims description 4
- 229940111688 monobasic potassium phosphate Drugs 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 150000003112 potassium compounds Chemical class 0.000 claims description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical class [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000013078 crystal Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 6
- -1 hydrogen fluoride anhydride Chemical class 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical compound [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Description
【発明の詳細な説明】
〔産業上の利用分野〕
６−フツ化りん酸カリウムは６−フツ化りん酸
ジアゾニウム化合物の製造原料やPF5の原料とし
て用いられる。とくに６−フツ化りん酸ジアゾニ
ウム化合物は熱安定性がよく、フアクシミリの感
熱記録紙の発色材料として利用されている。[Detailed Description of the Invention] [Industrial Application Field] Potassium 6-fluorophosphate is used as a raw material for producing 6-fluorophosphate diazonium compounds and as a raw material for PF 5 . In particular, diazonium 6-fluorophosphate compounds have good thermal stability and are used as coloring materials for thermosensitive recording paper for facsimiles.
〔従来の技術〕と〔発明が解決しようとする問題
点〕
６−フツ化りん酸カリウムは、(1)無水フツ化水
素酸の存在下、塩化カリウムと五塩化りんとを反
応させることにより製造するか、(2)無水フツ化水
素酸に五酸化りんを反応させて６−フツ化りん酸
溶液を製造後、フツ化カリウムや水酸化カリウム
等のカリウム塩を反応させて製造する方法があ
る。[Prior art] and [Problems to be solved by the invention] 6-Potassium fluorophosphate is produced by (1) reacting potassium chloride and phosphorus pentachloride in the presence of anhydrous hydrofluoric acid. Alternatively, (2) there is a method in which anhydrous hydrofluoric acid is reacted with phosphorus pentoxide to produce a 6-fluorinated phosphoric acid solution, and then a potassium salt such as potassium fluoride or potassium hydroxide is reacted with the solution.
(1)の方法はWoyski M.M.、“Inorganic
Syntheses”、vol、III、p.111（1950）New
York、Tronto、Londonに記載されている。こ
の方法では五塩化りんという吸湿性で発煙性の固
体を用いると共に、反応時塩化水素ガスが発生す
るため、その除外をしなければならないなど作業
性が悪いという欠点を有している。(2)の反応は
USP2488299に記載されており、反応性が激し
く、しかも吸湿性の強い五酸化りんを扱うという
作業性の悪い欠点を有している。 Method (1) is described by Woyski MM, “Inorganic
Syntheses”, vol, III, p.111 (1950) New
Listed in York, Toronto, and London. This method uses phosphorus pentachloride, a hygroscopic and fuming solid, and has the disadvantage of poor workability, such as the fact that hydrogen chloride gas is generated during the reaction and must be removed. The reaction of (2) is
It is described in USP 2488299, and has the disadvantage of poor workability as it involves handling highly reactive and hygroscopic phosphorus pentoxide.
〔問題点を解決するための手段〕と〔作用〕
本発明は、公知の方法とは異なる、新規で作業
性の良い６−フツ化りん酸カリウムの製造方法に
関する。[Means for Solving the Problems] and [Operation] The present invention relates to a novel method for producing potassium 6-fluorophosphate, which is different from known methods and has good workability.
本発明者らは６−フツ化りん酸カリウムの製造
方法について多数の研究を行つた結果、原料とし
て第一りん酸カリウムまたはポリリン酸カリウム
を用いて、これとフツ化水素酸または無水フツ化
水素酸と反応させることによつて６−フツ化りん
酸カリウムが効率良く得られることを見出したの
である。この第一りん酸カリウムまたはポリリン
酸カリウムは五塩化りんや無水五酸化りんと異な
り、発煙性や吸湿性がなく取り扱い易い原料であ
り、作業性にもすぐれている。 The present inventors have conducted numerous studies on the production method of 6-fluoropotassium phosphate, and as a result, using monopotassium phosphate or potassium polyphosphate as a raw material, it is combined with hydrofluoric acid or hydrogen fluoride anhydride. They discovered that 6-fluoropotassium phosphate can be efficiently obtained by reacting with an acid. Unlike phosphorus pentachloride or anhydrous phosphorus pentoxide, this monobasic potassium phosphate or potassium polyphosphate is an easy-to-handle raw material that does not emit smoke or absorb moisture, and has excellent workability.
フツ化水素酸または無水フツ化水素酸は反応物
質であると共に、溶媒として用いられる。フツ化
水素酸のHF濃度は60〜97重量％、好ましくは70
〜85重量％のものが用いられる。無水フツ化水素
酸はHF濃度が97重量％以上、好ましくは99重量
％以上のものが用いられる。 Hydrofluoric acid or hydrofluoric anhydride is both a reactant and a solvent. The HF concentration of hydrofluoric acid is 60-97% by weight, preferably 70
~85% by weight is used. Hydrofluoric anhydride having an HF concentration of 97% by weight or more, preferably 99% by weight or more is used.
反応容器はフツ化水素酸を用いる場合は、テフ
ロン、塩化ビニルまたはポリエチレン製のものま
たはこれらでライニングされたものを使用し、無
水フツ化水素酸の場合はニツケル、モネルメタ
ル、ハステロイメタルまたはステンレススチール
などの耐食材料でつくられたものを使用する。 When using hydrofluoric acid, the reaction vessel should be made of or lined with Teflon, vinyl chloride, or polyethylene; when using hydrofluoric anhydride, it should be made of nickel, Monel metal, Hastelloy metal, or stainless steel. Use materials made from corrosion-resistant materials.
反応はフツ化水素酸または無水フツ化水素酸を
５〜15℃に冷却し、撹拌しながらりん酸のカリウ
ム化合物をゆつくりと添加する。反応の進行と共
に溶液の温度が上昇するが、反応温度は70℃以
下、好ましくは50℃以下で行う。反応温度が70℃
以上になると、フツ化水素の飛散が起こり、収率
低下の原因となる。 In the reaction, hydrofluoric acid or anhydrous hydrofluoric acid is cooled to 5 to 15°C, and a potassium phosphoric acid compound is slowly added while stirring. Although the temperature of the solution increases as the reaction progresses, the reaction temperature is 70°C or lower, preferably 50°C or lower. Reaction temperature is 70℃
If the temperature exceeds that level, hydrogen fluoride will scatter, causing a decrease in yield.
りん酸のカリウム化合物の添加終了後、撹拌し
ながら冷却する。結晶を分離後、乾燥すれば高純
度の６−フツ化りん酸カリウムの無色柱状結晶が
得られる。 After the addition of the potassium phosphoric acid compound is complete, the mixture is cooled with stirring. After the crystals are separated and dried, highly pure colorless columnar crystals of potassium 6-fluorophosphate can be obtained.
本発明者は記述の本発明の方法に関して多数の
実験を行い、本発明の優秀性を確認したのである
が、更に本発明の技術的内容を明確にするため
に、代表的な例を抽出して以下に実施例として例
示する。従つて本発明の方法は以下に示された実
施例のみに限定して解釈されるべきではなく、任
意にその実施態様を変更し得ることは当然であ
る。
The present inventor conducted numerous experiments regarding the described method of the present invention and confirmed the superiority of the present invention, but in order to further clarify the technical content of the present invention, representative examples have been extracted. This will be illustrated below as an example. Therefore, the method of the present invention should not be construed as being limited to the examples shown below, and it is a matter of course that the embodiments can be changed as desired.
実施例 １
撹拌機付き、内容積９のハステロイＣ製反応
容器に99.9重量％無水フツ化水素酸4.9をいれ
て、５℃に冷却する。これに第一りん酸カリウム
3.5Kgを２時間で添加する。反応温度は10℃に保
つ。添加終了後２時間撹拌を続けた後、結晶を脱
水分離する。含水結晶を乾燥すれば、純度99.6％
の６−フツ化りん酸カリウム3.4Kg（収率72％）
が得られた。Example 1 4.9% of 99.9% by weight anhydrous hydrofluoric acid was placed in a Hastelloy C reaction vessel equipped with a stirrer and having an internal volume of 9, and cooled to 5°C. This includes monobasic potassium phosphate.
Add 3.5Kg in 2 hours. The reaction temperature is kept at 10°C. After the addition is complete, stirring is continued for 2 hours, and then the crystals are separated by dehydration. If the water-containing crystals are dried, the purity is 99.6%.
3.4Kg of 6-fluorinated potassium phosphate (yield 72%)
was gotten.
実施例 ２
撹拌機及び外部冷却ジヤケツト付きの塩化ビニ
ルライニングの反応容器に75重量％フツ化水素酸
を515Kg入れ、15℃に冷却する。撹拌しながら、
第一りん酸カリウム200Kgを２時間で添加する。
約70Kg添加した時反応温度は45℃に上昇、あとは
この温度を保つて反応させた。添加終了後、撹拌
しながら一夜放置して冷却した。結晶を脱水分離
し、含水結晶を乾燥すると、純度99.8％の６−フ
ツ化りん酸カリウム109Kg（収率41％）が得られ
た。Example 2 515 kg of 75% by weight hydrofluoric acid is placed in a vinyl chloride lined reaction vessel equipped with a stirrer and an external cooling jacket and cooled to 15°C. While stirring,
Add 200 kg of monobasic potassium phosphate in 2 hours.
When approximately 70 kg was added, the reaction temperature rose to 45°C, and the reaction was maintained at this temperature thereafter. After the addition was complete, the mixture was left to cool overnight while stirring. The crystals were dehydrated and separated, and the water-containing crystals were dried to obtain 109 kg of potassium 6-fluorophosphate with a purity of 99.8% (yield: 41%).
実施例 ３
撹拌機および冷却ジヤケツト付きテフロンライ
ニング反応器に80重量％フツ化水素酸47.4Kgを入
れ、15℃に冷却する。これにポリリン酸カリウム
16.0Kgを２時間で添加する。反応温度はポリリン
酸カリウム５Kg添加後、50℃に上昇、その後の反
応温度は50℃に保つた。添加終了後、撹拌しなが
ら、一夜放置して冷却した。結晶を脱水分離し、
含水結晶を乾燥すると、純度99.8％の６−フツ化
りん酸カリウム15.1Kg（収率62％）が得られた。Example 3 47.4 kg of 80% by weight hydrofluoric acid is placed in a Teflon-lined reactor equipped with a stirrer and cooling jacket and cooled to 15°C. Potassium polyphosphate
Add 16.0Kg in 2 hours. After adding 5 kg of potassium polyphosphate, the reaction temperature rose to 50°C, and thereafter the reaction temperature was maintained at 50°C. After the addition was complete, the mixture was left to cool overnight while stirring. Dehydrate and separate the crystals,
When the water-containing crystals were dried, 15.1 kg (yield: 62%) of 6-fluoropotassium phosphate with a purity of 99.8% was obtained.
本発明は以上説明した通りの６−フツ化りん酸
カリウムの製造方法であつて、取り扱いの容易な
りん酸のカリウム化合物が使用できることによつ
て、作業性良く高純度の６−フツ化りん酸カリウ
ムを製造することができる産業利用性の高い発明
である。
The present invention is a method for producing potassium 6-fluorophosphate as described above, and by using an easily handled potassium compound of phosphoric acid, it is possible to produce highly purified 6-fluorophosphate with good workability. This is a highly industrially applicable invention that can produce potassium.
Claims (1)
酸のカリウム化合物とを反応させることを特徴と
する６−フツ化りん酸カリウムの製造方法。 ２ りん酸のカリウム化合物が第一りん酸カリウ
ムまたはポリリン酸カリウムである特許請求の範
囲第１項記載の６−フツ化りん酸カリウムの製造
方法。 ３ フツ化水素酸がフツ化水素（HF）の濃度60
〜97重量％である特許請求の範囲第１項記載の６
−フツ化りん酸カリウムの製造方法。 ４ 無水フツ化水素酸がフツ化水素（HF）の濃
度97重量％以上である特許請求の範囲第１項記載
の６−フツ化りん酸カリウムの製造方法。[Scope of Claims] 1. A method for producing potassium 6-fluorophosphate, which comprises reacting hydrofluoric acid or hydrofluoric anhydride with a potassium compound of phosphoric acid. 2. The method for producing 6-fluoropotassium phosphate according to claim 1, wherein the potassium compound of phosphoric acid is monobasic potassium phosphate or potassium polyphosphate. 3 Hydrofluoric acid has a concentration of hydrogen fluoride (HF) of 60
~97% by weight 6 of claim 1
- A method for producing fluorinated potassium phosphate. 4. The method for producing 6-fluoropotassium phosphate according to claim 1, wherein the anhydrous hydrofluoric acid has a hydrogen fluoride (HF) concentration of 97% by weight or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19009086A JPS6345108A (en) | 1986-08-12 | 1986-08-12 | Production of potassium 6-fluorophosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19009086A JPS6345108A (en) | 1986-08-12 | 1986-08-12 | Production of potassium 6-fluorophosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6345108A JPS6345108A (en) | 1988-02-26 |
| JPH0572324B2 true JPH0572324B2 (en) | 1993-10-12 |
Family
ID=16252199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19009086A Granted JPS6345108A (en) | 1986-08-12 | 1986-08-12 | Production of potassium 6-fluorophosphate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6345108A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008096723A1 (en) | 2007-02-08 | 2008-08-14 | Stella Chemifa Corporation | Method for producing hexafluorophosphate salt |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100288825B1 (en) * | 1998-12-31 | 2001-05-02 | 박대치 | Method for producing lithium hexafluorophosphate |
| JP5351463B2 (en) | 2008-08-08 | 2013-11-27 | ステラケミファ株式会社 | Method for producing hexafluorophosphate |
| CN109422256A (en) * | 2017-08-28 | 2019-03-05 | 天津金牛电源材料有限责任公司 | A kind of preparation method of difluorophosphoric acid alkali metal salt |
-
1986
- 1986-08-12 JP JP19009086A patent/JPS6345108A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008096723A1 (en) | 2007-02-08 | 2008-08-14 | Stella Chemifa Corporation | Method for producing hexafluorophosphate salt |
| JP2008195547A (en) * | 2007-02-08 | 2008-08-28 | Stella Chemifa Corp | Method for producing hexafluorophosphate salt |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6345108A (en) | 1988-02-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |