CN101671037A - Method for preparing ammonium bifluoride with high purity - Google Patents
Method for preparing ammonium bifluoride with high purity Download PDFInfo
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- CN101671037A CN101671037A CN200910102716A CN200910102716A CN101671037A CN 101671037 A CN101671037 A CN 101671037A CN 200910102716 A CN200910102716 A CN 200910102716A CN 200910102716 A CN200910102716 A CN 200910102716A CN 101671037 A CN101671037 A CN 101671037A
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- ammonium bifluoride
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Abstract
The invention discloses a method for preparing an ammonium bifluoride with high purity. The ammonium fluoride with high purity is taken as a raw material and is decomposed at the temperature of 130-148.5 DEG C, thus generating ammonia gas; the ammonia gas generated by decomposition is absorbed by a dilute hydrochloric acid solution with the mass concentration of 5-12%; the ammonium fluoride crystals obtained by the decomposition are sublimed under the temperature of 222-230 DEG C; and the ammonium bifluoride vapor is collected, thus obtaining the ammonium bifluoride product. The method has high yield and high product purity and can meet high requirement.
Description
Technical field
The invention belongs to chemical field, relate in particular to a kind of preparation method of ammonium bifluoride with high purity.
Background technology
Ammonium bifluoride is a widely used class fluorine chemical product in the fluorine chemical industry, and ammonium bifluoride is white quadrature rhombus or plate crystal, relative density 1.5, and easy deliquescence is soluble in water in air, is slightly soluble in ethanol.Ammonium bifluoride is used for industry such as chemical industry, metallurgy, mechanical workout and food in a large number, and high-purity ammonium bifluoride also can be used for semi-conductor industry and medicine industry.
The production technique of ammonium bifluoride can be divided into vapor phase process and two kinds of methods of liquid phase method.The synthetic Neutral ammonium fluoride of vapor phase process is not because technological process contacts water, the product water content is low, purity can up to more than 99%, grain graininess is thin, can satisfy the requirement of electron trade and pharmaceutical industries, but vapor phase process is produced the Neutral ammonium fluoride stopping property very high to processing requirement, very high to equipment requirements, and investment is very big.Liquid phase method is because equipment is simple, and processing condition and operation of equipment are easy to control and are used widely, and the domestic liquid phase method that generally adopts prepares ammonium bifluoride at present.But the ammonium bifluoride water content height of liquid phase method preparation, purity generally less than 97%, phenomenons such as moisture absorption caking can appear in standing storage, can not adapt to the needs of industries such as the electronic industry of having relatively high expectations, medicine industry, only can reach the technical grade requirement usually.
Summary of the invention
A kind of rate of recovery height that the objective of the invention is to overcome above-mentioned shortcoming and provide, product purity are high and can satisfy the preparation method of the ammonium bifluoride with high purity of high requirement.
The invention provides a kind of preparation method of ammonium bifluoride with high purity, be to be raw material with the ammonium fluoride with high purity, between 130-148.5 ℃ ammonium fluoride with high purity is decomposed, decomposition obtains the ammonium bifluoride crystal and distils between 222-230 ℃, collects the ammonium bifluoride steam and obtains the ammonium bifluoride with high purity product.
The preparation method of above-mentioned a kind of ammonium bifluoride with high purity, wherein: the ammonia mass concentration of decomposing generation is that the dilute hydrochloric acid solution of 5-12% absorbs.
The preparation method of above-mentioned a kind of ammonium bifluoride with high purity, wherein: decomposition temperature is between 135-148.5 ℃ the time, and the decomposition effect of Neutral ammonium fluoride is best.
The preparation method of above-mentioned a kind of ammonium bifluoride with high purity, wherein: when ammonium bifluoride crystalline sublimation temperature is controlled between 222-225 ℃, can guarantee the efficient distillation of ammonium bifluoride.
The present invention compared with prior art, as can be known from the above technical solutions, with the ammonium fluoride with high purity is raw material, saved the purification step of preparation ammonium bifluoride with high purity raw material, simultaneously reasonably control Neutral ammonium fluoride and prepared the decomposition temperature of ammonium bifluoride and the sublimation temperature of ammonium bifluoride, when reducing decomposition and distillation energy consumption, guaranteed the quality purity of ammonium bifluoride product.
Below, further specify beneficial effect of the present invention by embodiment.
Embodiment
Embodiment 1
Get the 500g ammonium fluoride with high purity, under 130 ℃ ammonium fluoride with high purity is decomposed, the ammonia mass concentration that decompose to produce is that 5% dilute hydrochloric acid solution absorbs; Decompose the ammonium bifluoride crystal that obtains and distil at 222 ℃, it is 99.1% ammonium bifluoride with high purity product that collection ammonium bifluoride steam obtains mass content.
Embodiment 2
Get the 600g ammonium fluoride with high purity, under 135 ℃ ammonium fluoride with high purity is decomposed, decomposing the ammonia mass concentration that produces is that 6% dilute hydrochloric acid solution absorbs; Decompose the ammonium bifluoride crystal that obtains and distil at 224 ℃, it is 99.2% ammonium bifluoride with high purity product that collection ammonium bifluoride steam obtains mass content.
Embodiment 3
Get the 450g ammonium fluoride with high purity, under 139 ℃ ammonium fluoride with high purity is decomposed, decomposing the ammonia mass concentration that produces is that 8% dilute hydrochloric acid solution absorbs; Decompose the ammonium bifluoride crystal that obtains and distil at 225 ℃, it is 98.9% ammonium bifluoride with high purity product that collection ammonium bifluoride steam obtains mass content.
Embodiment 4
Get the 650g ammonium fluoride with high purity, under 143 ℃ ammonium fluoride with high purity is decomposed, decomposing the ammonia mass concentration that produces is that 10% dilute hydrochloric acid solution absorbs; Decomposition obtains the ammonium bifluoride crystal and distils at 228 ℃, and it is 99.1% ammonium bifluoride with high purity product that collection ammonium bifluoride steam obtains mass content.
Embodiment 5
Get the 700g ammonium fluoride with high purity, under 148.5 ℃ ammonium fluoride with high purity is decomposed, decomposing the ammonia mass concentration that produces is that 12% dilute hydrochloric acid solution absorbs; Decomposition obtains the ammonium bifluoride crystal and distils at 230 ℃, and it is 98.8% ammonium bifluoride with high purity product that collection ammonium bifluoride steam obtains mass content.
The quality product of embodiment 1-5 sees the following form:
| Embodiment | ??1 | ??2 | ??3 | ??4 | ??5 |
| Content (NH 4HF 2)％ | ??99.1 | ??99.2 | ??98.9 | ??99.1 | ??98.8 |
| Ignition residue (in vitriol) % | ??0.007 | ??0.006 | ??0.004 | ??0.005 | ??0.008 |
| Muriate (Cl) % | ??0.0008 | ??0.0007 | ??0.0005 | ??0.0009 | ??0.001 |
| Silicofluoride (SiF 6)％ | ??0.09 | ??0.08 | ??0.04 | ??0.1 | ??0.09 |
| Vitriol (SO 4)％ | ??0.0047 | ??0.0042 | ??0.0039 | ??0.0035 | ??0.0046 |
| Iron (Fe) % | ??0.00065 | ??0.00074 | ??0.00058 | ??0.00057 | ??0.00081 |
| Heavy metal (in Pb) % | ??0.0012 | ??0.0026 | ??0.0011 | ??0.0015 | ??0.002 |
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (4)
1, a kind of preparation method of ammonium bifluoride with high purity, it is characterized in that: in temperature is between 130-148.5 ℃ ammonium fluoride with high purity to be decomposed, it is to distil between 222-230 ℃ in temperature that decomposition obtains the ammonium bifluoride crystal, collects the ammonium bifluoride steam and obtains the ammonium bifluoride with high purity product.
2, the preparation method of a kind of ammonium bifluoride with high purity as claimed in claim 1 is characterized in that: the ammonia mass concentration of decomposing generation is that the dilute hydrochloric acid solution of 5-12% absorbs.
3, the preparation method of a kind of ammonium bifluoride with high purity as claimed in claim 1 or 2 is characterized in that: decomposition temperature is 135-148.5 ℃.
4, the preparation method of a kind of ammonium bifluoride with high purity as claimed in claim 3 is characterized in that: ammonium bifluoride crystalline sublimation temperature is controlled to be 222-225 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200910102716A CN101671037A (en) | 2009-08-03 | 2009-08-03 | Method for preparing ammonium bifluoride with high purity |
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| CN200910102716A CN101671037A (en) | 2009-08-03 | 2009-08-03 | Method for preparing ammonium bifluoride with high purity |
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| CN101671037A true CN101671037A (en) | 2010-03-17 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121664A (en) * | 2012-12-21 | 2013-05-29 | 山东兴氟新材料有限公司 | Production technique of high-purity hydrofluoric acid |
| CN103121699A (en) * | 2013-02-26 | 2013-05-29 | 贵州金正大生态工程有限公司 | Method for preparing potassium fluoride by utilizing potassium fluosilicate |
| CN103219052A (en) * | 2013-04-25 | 2013-07-24 | 中国科学院上海有机化学研究所 | Highly purified fluoride fused salt and preparation method thereof |
| CN113479908A (en) * | 2021-07-15 | 2021-10-08 | 江西省东沿药业有限公司 | Preparation method of ammonium fluoride or ammonium bifluoride |
| CN115676851A (en) * | 2022-11-23 | 2023-02-03 | 贵州省化工研究院 | Method and device for preparing ammonium bifluoride from solid ammonium fluoride |
-
2009
- 2009-08-03 CN CN200910102716A patent/CN101671037A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121664A (en) * | 2012-12-21 | 2013-05-29 | 山东兴氟新材料有限公司 | Production technique of high-purity hydrofluoric acid |
| CN103121699A (en) * | 2013-02-26 | 2013-05-29 | 贵州金正大生态工程有限公司 | Method for preparing potassium fluoride by utilizing potassium fluosilicate |
| CN103121699B (en) * | 2013-02-26 | 2017-03-01 | 金正大诺泰尔化学有限公司 | A kind of method that potassium fluosilicate prepares potassium fluoride |
| CN103219052A (en) * | 2013-04-25 | 2013-07-24 | 中国科学院上海有机化学研究所 | Highly purified fluoride fused salt and preparation method thereof |
| CN103219052B (en) * | 2013-04-25 | 2016-04-13 | 中国科学院上海有机化学研究所 | A kind of highly purified fluoride molten salt and preparation method thereof |
| CN113479908A (en) * | 2021-07-15 | 2021-10-08 | 江西省东沿药业有限公司 | Preparation method of ammonium fluoride or ammonium bifluoride |
| CN115676851A (en) * | 2022-11-23 | 2023-02-03 | 贵州省化工研究院 | Method and device for preparing ammonium bifluoride from solid ammonium fluoride |
| CN115676851B (en) * | 2022-11-23 | 2024-05-21 | 贵州省化工研究院 | Method and device for preparing ammonium bifluoride from solid ammonium fluoride |
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Open date: 20100317 |