CN105819463A - Synthesis method of ferrous tetrafluoroborate - Google Patents
Synthesis method of ferrous tetrafluoroborate Download PDFInfo
- Publication number
- CN105819463A CN105819463A CN201610271010.8A CN201610271010A CN105819463A CN 105819463 A CN105819463 A CN 105819463A CN 201610271010 A CN201610271010 A CN 201610271010A CN 105819463 A CN105819463 A CN 105819463A
- Authority
- CN
- China
- Prior art keywords
- ferrous
- iron powder
- fluoboric acid
- synthetic method
- acid
- 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.)
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- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000001308 synthesis method Methods 0.000 title abstract 3
- -1 tetrafluoroborate Chemical compound 0.000 title abstract 3
- 239000002253 acid Substances 0.000 claims abstract description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000047 product Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000010189 synthetic method Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- NNBFNNNWANBMTI-UHFFFAOYSA-M brilliant green Chemical compound OS([O-])(=O)=O.C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 NNBFNNNWANBMTI-UHFFFAOYSA-M 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 241000579895 Chlorostilbon Species 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229910052876 emerald Inorganic materials 0.000 abstract 1
- 239000010976 emerald Substances 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000012491 analyte Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229960002089 ferrous chloride Drugs 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005323 electroforming Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical group O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a synthesis method of ferrous tetrafluoroborate. The synthesis method comprises the following steps: proportionally weighing iron powder and fluoboric acid, adding the fluoboric acid liquid into a reactor, and slowly adding the iron powder into the fluoboric acid solution while continuously stirring; when the reaction proceeds slowly, heating to continue the reaction; and after the reaction finishes, filtering the obtained emerald suspension, carrying out evaporative concentration on the obtained solution, standing the obtained suspension, sufficiently crystallizing and precipitating, filtering the obtained product, and drying the filtered substance to obtain the final product. The technique is simple and reasonable, has the advantages of low energy consumption, low pollution and greatly higher yield, and provides a ferrous tetrafluoroborate preparation method which is simple to operate and friendly to the environment.
Description
Technical field
The present invention relates to inorganic chemical industry synthesis field, the synthetic method that a kind of Tetrafluoroboric acid is ferrous.
Background technology
Tetrafluoroboric acid ferrous iron can be used for making electroplate liquid, plating iron layer plating of practicality as economy.The iron layer purity of plating is high, the most wear-resisting, easy melting welding, is mainly used in the bent axle of wearing part such as automobile, locomotive and the reparation of heavy duty machine tools wear-out part and the electroforming of mould.Iron plating is also used as the intermediate layer before ironcasting electrogalvanizing, stannum, chromium or the intermediate layer before galvanizing.The plating solution of current wide use is copperas solution, solution of ferrous chloride or the solution of both mixing.But in the system of Tetrafluoroboric acid ferrous iron solution, during plating iron, can get the plating iron layer of fine uniform, thus Tetrafluoroboric acid ferrous iron solution has certain application potential in modern electroplating technology field.Tetrafluoroboric acid ferrous iron solution has good stability, high conductivity and the high tolerance to metal impurities.Antioxygenic property and the acidity shock-absorbing capacity of the most this plating solution are all significantly increased, and be no longer necessary to energising and process and adjust acidity in production.The dispersibility of plating solution and once plating thickness ability relatively solution of ferrous chloride increase, and owing to acidity is low, hydrogen is difficult to separate out at negative electrode, and coating hydrogen content is few, so fragility is little, adhesion is strong, and quality is more stable.The preparation that Tetrafluoroboric acid is ferrous at present also uses general Inorganic synthese mode to be prepared, this preparation method, and energy consumption is high, and productivity is low, pollutes the biggest.
Summary of the invention
It is an object of the invention to provide the synthetic method that a kind of Tetrafluoroboric acid is ferrous, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
The synthetic method that a kind of Tetrafluoroboric acid is ferrous, specifically comprises the following steps that
(1) iron powder, fluoboric acid are weighed the most respectively；
(2) fluoboric acid liquid is joined in reactor, iron powder is slowly added in fluoborate solution, the most constantly stirring；
(3), when question response carries out slow, heating proceeds reaction, and reaction temperature controls for 55～65 DEG C, and the response time is 90～360min；
(4), after having reacted, the emerald green suspension obtained is filtered；
(5) it is evaporated filtration gained solution concentrating；
(6) being stood by the suspension concentrating gained, sufficient crystallising precipitates；
(7) being filtered by crystallization products therefrom, taking screening is dried, and obtains final products.
As the further scheme of the present invention: in described step (1), iron powder is 1.1～1.2:2 with the mol ratio of fluoboric acid.
As the further scheme of the present invention: in described step (5), evaporation and concentration is carried out at vacuum condition, evaporating temperature is 55～68 DEG C.
As the present invention further scheme: in described step (7), being dried and carry out under vacuum, baking temperature is 30～45 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: the inventive method technique advantages of simple, energy consumption is low, pollutes little, and productivity is also greatly improved, and the preparation ferrous for Tetrafluoroboric acid provides a kind of method being simple to operate and friendly to environment.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
The synthesis step of Tetrafluoroboric acid ferrous iron is as follows:
(1) weighing iron powder, fluoboric acid the most respectively, iron powder is 1.1:2 with the mol ratio of fluoboric acid；
(2) fluoboric acid liquid is joined in reactor, iron powder is slowly added in fluoborate solution, the most constantly stirring；
(3), when question response carries out slow, heating proceeds reaction, and reaction temperature controls for 65 DEG C, and the response time is 90min；
(4), after having reacted, the emerald green suspension obtained is filtered；
(5) being evaporated filtration gained solution under vacuum concentrating, evaporating temperature is 55 DEG C；
(6) being stood by the suspension concentrating gained, sufficient crystallising precipitates；
(7) being filtered by crystallization products therefrom, taking screening is dried under vacuum, and baking temperature is 30 DEG C, obtains final products.
Final products are light green color crystalline particle, are consistent product standard PDF card through XRD detection analyte, and productivity is 95.6%.
Embodiment 2
The Hydrothermal Synthesis step of Tetrafluoroboric acid ferrous iron is as follows:
(1) weighing iron powder, fluoboric acid the most respectively, iron powder is 1.15:2 with the mol ratio of fluoboric acid；
(2) fluoboric acid liquid is joined in reactor, iron powder is slowly added in fluoborate solution, the most constantly stirring；
(3), when question response carries out slow, heating proceeds reaction, and reaction temperature controls for 55 DEG C, and the response time is 180min；
(4), after having reacted, the emerald green suspension obtained is filtered；
(5) being evaporated filtration gained solution under vacuum concentrating, evaporating temperature is 62 DEG C；
(6) being stood by the suspension concentrating gained, sufficient crystallising precipitates；
(7) being filtered by crystallization products therefrom, taking screening is dried under vacuum, and baking temperature is 38 DEG C and obtains final products.
Final products are light green color crystalline particle, are consistent product standard PDF card through XRD detection analyte, and productivity is 96%.
Embodiment 3
The Hydrothermal Synthesis step of Tetrafluoroboric acid ferrous iron is as follows:
(1) weighing iron powder, fluoboric acid the most respectively, iron powder is 1.2:2 with the mol ratio of fluoboric acid；
(2) fluoboric acid liquid is joined in reactor, iron powder is slowly added in fluoborate solution, the most constantly stirring；
(3), when question response carries out slow, heating proceeds reaction, and reaction temperature controls for 56 DEG C, and the response time is 360min；
(4), after having reacted, the emerald green suspension obtained is filtered；
(5) being evaporated filtration gained solution under vacuum concentrating, evaporating temperature is 68 DEG C；
(6) being stood by the suspension concentrating gained, sufficient crystallising precipitates；
(7) being filtered by crystallization products therefrom, taking screening is dried under vacuum, and baking temperature is 45 DEG C, obtains final products.
Final products are light green color crystalline particle, are consistent product standard PDF card through XRD detection analyte, and productivity is 95.4%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and without departing from the spirit or essential characteristics of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is limited by claims rather than described above, it is intended that all changes fallen in the implication of equivalency and scope of claim included in the present invention.
Claims (4)
1. the synthetic method that a Tetrafluoroboric acid is ferrous, it is characterised in that specifically comprise the following steps that
(1) iron powder, fluoboric acid are weighed the most respectively；
(2) fluoboric acid liquid is joined in reactor, iron powder is slowly added in fluoborate solution, the most constantly stirring；
(3), when question response carries out slow, heating proceeds reaction, and reaction temperature controls for 55～65 DEG C, and the response time is 90～360min；
(4), after having reacted, the emerald green suspension obtained is filtered；
(5) it is evaporated filtration gained solution concentrating；
(6) being stood by the suspension concentrating gained, sufficient crystallising precipitates；
(7) being filtered by crystallization products therefrom, taking screening is dried, and obtains final products.
The synthetic method that Tetrafluoroboric acid the most according to claim 1 is ferrous, it is characterised in that in described step (1), iron powder is 1.1～1.2:2 with the mol ratio of fluoboric acid.
The synthetic method that Tetrafluoroboric acid the most according to claim 1 is ferrous, it is characterised in that in described step (5), evaporation and concentration is carried out at vacuum condition, and evaporating temperature is 55～68 DEG C.
The synthetic method that Tetrafluoroboric acid the most according to claim 1 is ferrous, it is characterised in that in described step (7), is dried and carries out under vacuum, and baking temperature is 30～45 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610271010.8A CN105819463A (en) | 2016-04-27 | 2016-04-27 | Synthesis method of ferrous tetrafluoroborate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610271010.8A CN105819463A (en) | 2016-04-27 | 2016-04-27 | Synthesis method of ferrous tetrafluoroborate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105819463A true CN105819463A (en) | 2016-08-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610271010.8A Pending CN105819463A (en) | 2016-04-27 | 2016-04-27 | Synthesis method of ferrous tetrafluoroborate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105819463A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5372684A (en) * | 1992-06-03 | 1994-12-13 | Ecochem Aktiengesellschaft | Process for the direct electrochemical refining of copper scrap |
| CN1762979A (en) * | 2005-09-26 | 2006-04-26 | 陈耀华 | Tetraethyl tetrafluo ammonium fluoroborate preparation method |
-
2016
- 2016-04-27 CN CN201610271010.8A patent/CN105819463A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5372684A (en) * | 1992-06-03 | 1994-12-13 | Ecochem Aktiengesellschaft | Process for the direct electrochemical refining of copper scrap |
| CN1762979A (en) * | 2005-09-26 | 2006-04-26 | 陈耀华 | Tetraethyl tetrafluo ammonium fluoroborate preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 姚守拙等: "《元素化学反应手册》", 31 July 1998 * |
| 李英春: "《氟化合物制备及应用》", 31 August 2010 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20160803 |