CN112960678A - Method for removing crystal water and purifying crude silver tetrafluoroborate - Google Patents
Method for removing crystal water and purifying crude silver tetrafluoroborate Download PDFInfo
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- CN112960678A CN112960678A CN202110165728.XA CN202110165728A CN112960678A CN 112960678 A CN112960678 A CN 112960678A CN 202110165728 A CN202110165728 A CN 202110165728A CN 112960678 A CN112960678 A CN 112960678A
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- silver tetrafluoroborate
- water
- anhydrous
- acetonitrile
- crude
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- -1 silver tetrafluoroborate Chemical compound 0.000 title claims abstract description 63
- 229910001494 silver tetrafluoroborate Inorganic materials 0.000 title claims abstract description 63
- 239000013078 crystal Substances 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 29
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 9
- 208000005156 Dehydration Diseases 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 150000001350 alkyl halides Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910001923 silver oxide Inorganic materials 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001351 alkyl iodides Chemical class 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Chemical group C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 150000001541 aziridines Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012038 nucleophile Substances 0.000 description 1
- 239000012434 nucleophilic reagent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000006462 rearrangement reaction Methods 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- 229940096017 silver fluoride Drugs 0.000 description 1
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a method for removing crystal water from crude silver tetrafluoroborate and purifying the crude silver tetrafluoroborate, and high-purity anhydrous silver tetrafluoroborate can be obtained after the crude silver tetrafluoroborate is treated by the method. The method takes a crude product of the silver tetrafluoroborate containing crystal water prepared in an aqueous solution medium system as a raw material, the crude product of the silver tetrafluoroborate is dissolved in dehydrated anhydrous acetonitrile, insoluble impurities are removed by filtration, filtrate is collected and subjected to vacuum concentration, wherein water and the acetonitrile form an azeotrope and are distilled and separated, and then the water and the acetonitrile are fully subjected to vacuum concentration at a higher temperature so as to be completely separated from the water and the acetonitrile. The method is characterized in that the removal of the silver tetrafluoroborate crystal water is carried out in an organic medium system, water or a water-containing reagent is not introduced, and the anhydrous silver tetrafluoroborate without crystal water is prepared after treatment. The purification method is simple to operate, mild in operation conditions and high in yield, and ensures that high-quality anhydrous silver tetrafluoroborate is obtained, and the product meets the market demand.
Description
Technical Field
The invention relates to a method for removing crystal water and purifying crude silver tetrafluoroborate, which can obtain high-purity anhydrous silver tetrafluoroborate after being treated by the method.
Technical Field
Silver tetrafluoroborate, also called silver tetrafluoroborate, has a molecular formula of AgBF4It is white crystal solid, easy to absorb moisture, and has good water solubility, and can be dissolved in organic solvent such as benzene and ethyl ether.
Silver tetrafluoroborate is a weak lewis acid, has a particular affinity for organic halides, and can be widely used as a homogeneous catalyst. Under the catalytic action of silver tetrafluoroborate, nucleophilic reagent can perform nucleophilic substitution reaction on alkyl halide, and similar reaction is used for synthesizing indole alkaloid skeleton compounds; for nitrogen nucleophiles, nucleophilic substitution of alkyl halides can also be carried out, for example, intramolecular reaction of tertiary amines with alkyl iodides to form aziridine salts. In addition, the alkyl halides can be converted to the corresponding alcohols under the catalysis of silver tetrafluoroborate, and some alkyl halides can also undergo rearrangement reactions. In addition, silver tetrafluoroborate can be used in organic synthesis reactions in addition to catalyzing nucleophilic substitution reactions, as an anion-converting reagent to provide tetrafluoroborate. With the continuous and deep research of organic synthesis reaction, the application field of silver tetrafluoroborate as a catalyst or an auxiliary agent in the organic synthesis reaction is continuously expanded. Most of the synthesis reactions must be operated under anhydrous conditions, the water content of the reaction system is strictly controlled, and the catalyst, the auxiliary agent and the like added in the reaction process cannot contain water. Therefore, the moisture-free high-quality silver tetrafluoroborate has better application prospect and high market price.
The silver tetrafluoroborate without crystal water can be prepared by reacting silver fluoride with gaseous boron trifluoride, but the anhydrous silver tetrafluoroborate prepared by the method is expensive due to the limitation of raw material price. The silver tetrafluoroborate is synthesized by the reaction of silver carbonate (or silver oxide) and hydrofluoric acid, the synthesis method is simple and easy to implement, but the reaction system is an aqueous medium, the prepared silver tetrafluoroborate has crystal water, the use is limited, and the product has no competitive advantage if the crystal water is not removed. The crystal water of the compound is present in the crystal, and is not liquid water, and can be removed by thermal decomposition, use of a dehydrating agent, storage in a dry atmosphere, or the like. Thermal decomposition is the most commonly used method for removing crystal water, but the method is not suitable for removing crystal water of silver tetrafluoroborate, because silver tetrafluoroborate is unstable under the action of water during heating and is partially decomposed into grey black silver oxide, and high-purity white anhydrous silver tetrafluoroborate cannot be obtained.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for removing silver tetrafluoroborate crystal water, which is to treat a crude product of silver tetrafluoroborate prepared in an aqueous solution medium system to obtain high-quality anhydrous silver tetrafluoroborate. The method is simple to operate, high in yield, capable of ensuring that the high-quality anhydrous silver tetrafluoroborate can be obtained, reducing the production cost, and the product meets the market demand.
In order to effectively remove crystal water in the silver tetrafluoroborate and obtain anhydrous silver tetrafluoroborate, the invention adopts the following technical scheme:
a method for removing crystal water and purifying crude silver tetrafluoroborate comprises the following steps:
step (1), dissolving a crude product of silver tetrafluoroborate in anhydrous acetonitrile subjected to pre-dehydration treatment, heating in a dark place, stirring until the silver tetrafluoroborate is completely dissolved, and filtering to remove insoluble impurities to obtain a filtrate A;
step (2), concentrating the filtrate A in vacuum until the solvent is evaporated until white crystals are separated out;
and (3) raising the temperature, continuing to concentrate until no solvent is evaporated, cooling to room temperature in a vacuum state, and collecting white crystals which are anhydrous silver tetrafluoroborate.
Preferably, the preparation method of the anhydrous acetonitrile subjected to the pre-dehydration treatment in the step (1) comprises the following steps: and dehydrating the commercially available acetonitrile by adopting a molecular sieve to prepare the anhydrous acetonitrile.
Preferably, the heating temperature in the step (1) is 40-60 ℃.
Preferably, the use amount of the anhydrous acetonitrile in the step (1) is 4-10 ml of anhydrous acetonitrile correspondingly added to each gram of the crude silver tetrafluoroborate.
Preferably, the vacuum concentration in the step (2) is carried out under the conditions that the vacuum degree is 0.04-0.08 MPa and the temperature is 50-75 ℃.
Preferably, the temperature for continuously concentrating at the high temperature in the step (3) is 120-140 ℃.
The method takes a crude product of the silver tetrafluoroborate containing crystal water prepared in an aqueous solution medium system as a raw material, the crude product of the silver tetrafluoroborate is dissolved in dehydrated anhydrous acetonitrile, insoluble impurities are removed by filtration, filtrate is collected and subjected to vacuum concentration, wherein water and the acetonitrile form an azeotrope and are distilled and separated, and then the water and the acetonitrile are fully subjected to vacuum concentration at a higher temperature so as to completely remove the water and the acetonitrile. The method has the advantages of mild operation conditions, simple and easily realized process, high purification yield and capability of obtaining the high-quality anhydrous silver tetrafluoroborate.
The invention also has the following unique advantages:
(1) the method can purify and treat the crude product of the silver tetrafluoroborate synthesized in the aqueous solution medium system, thereby greatly reducing the production cost of the anhydrous silver tetrafluoroborate;
(2) the method for removing the crystal water does not introduce a water-containing solvent, and ensures that high-quality anhydrous silver tetrafluoroborate is obtained;
(3) the invention has mild operation condition, simple and easily realized process and high yield up to over 80 percent.
Detailed Description
For a better understanding and an enabling practice of the present invention, the present invention is further illustrated below by reference to specific examples, but is not limited to the methods described in the examples.
Example 1
Taking 10.05 g of crude silver tetrafluoroborate, adding the crude silver tetrafluoroborate into a flask, pouring 40mL of anhydrous acetonitrile subjected to pre-dehydration treatment, heating to 40 ℃, stirring, filtering to remove insoluble impurities, and collecting filtrate; vacuum concentrating the filtrate at 50 deg.C under 0.08MPa, evaporating the solvent until white crystal is separated out, heating to 120 deg.C, cooling to room temperature under vacuum, filtering, and collecting white crystal; 8.16 g of a white solid was obtained, which was determined to be anhydrous silver tetrafluoroborate by silver content analysis and infrared spectroscopic analysis, with a yield of 81.2%.
Example 2
Taking 10.01 g of crude silver tetrafluoroborate, adding the crude silver tetrafluoroborate into a flask, pouring 60mL of anhydrous acetonitrile subjected to pre-dehydration treatment, heating to 50 ℃, stirring, filtering to remove insoluble impurities, and collecting filtrate; vacuum concentrating the filtrate at 60 deg.C under 0.04MPa, evaporating the solvent until white crystal is separated out, heating to 130 deg.C, cooling to room temperature under vacuum, filtering, and collecting white crystal; 8.23 g of a white solid was obtained, which was determined to be anhydrous silver tetrafluoroborate by silver content analysis and infrared spectroscopic analysis, with a yield of 82.9%.
Example 3
Taking 10.12 g of crude silver tetrafluoroborate, adding the crude silver tetrafluoroborate into a flask, pouring 80mL of anhydrous acetonitrile subjected to pre-dehydration treatment, heating to 60 ℃, stirring, filtering to remove insoluble impurities, and collecting filtrate; vacuum concentrating the filtrate at 75 deg.C under 0.06MPa, evaporating the solvent until white crystal is separated out, heating to 135 deg.C, cooling to room temperature under vacuum, filtering, and collecting white crystal; 8.18 g of a white solid was obtained, which was determined to be anhydrous silver tetrafluoroborate by silver content analysis and infrared spectroscopic analysis, with a yield of 80.8%.
Example 4
Taking 10.08 g of crude silver tetrafluoroborate, adding the crude silver tetrafluoroborate into a flask, pouring 100mL of anhydrous acetonitrile subjected to pre-dehydration treatment, heating to 55 ℃, stirring, filtering to remove insoluble impurities, and collecting filtrate; vacuum concentrating the filtrate at 55 deg.C under 0.08MPa, evaporating the solvent until white crystal is separated out, heating to 130 deg.C, cooling to room temperature under vacuum, filtering, and collecting white crystal; 8.27 g of a white solid was obtained, which was determined to be anhydrous silver tetrafluoroborate by silver content analysis and infrared spectroscopic analysis, with a yield of 82.0%.
Claims (6)
1. A method for removing crystal water and purifying crude silver tetrafluoroborate is characterized by comprising the following steps:
step (1), dissolving a crude product of silver tetrafluoroborate in anhydrous acetonitrile subjected to pre-dehydration treatment, heating in a dark place, stirring until the silver tetrafluoroborate is completely dissolved, and filtering to remove insoluble impurities to obtain a filtrate A;
step (2), concentrating the filtrate A in vacuum until the solvent is evaporated until white crystals are separated out;
and (3) raising the temperature, continuing to concentrate until no solvent is evaporated, cooling to room temperature in a vacuum state, and collecting white crystals which are anhydrous silver tetrafluoroborate.
2. The method of claim 1, wherein:
the heating temperature in the step (1) is 40-60 ℃.
3. The method of claim 1, wherein:
and (2) the consumption of the anhydrous acetonitrile in the step (1) is that 4-10 ml of anhydrous acetonitrile is correspondingly added into each gram of the crude silver tetrafluoroborate.
4. The method of claim 1, wherein:
and (3) performing vacuum concentration in the step (2) under the conditions that the vacuum degree is 0.04-0.08 MPa and the temperature is 50-75 ℃.
5. The method of claim 1, wherein:
and (4) continuously concentrating at the high temperature in the step (3) at 120-140 ℃.
6. The process according to any one of claims 1 to 5, wherein the method for pre-dehydration treatment of anhydrous acetonitrile in step (1) is:
and dehydrating the commercially available acetonitrile by adopting a molecular sieve to prepare the anhydrous acetonitrile.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110165728.XA CN112960678A (en) | 2021-02-06 | 2021-02-06 | Method for removing crystal water and purifying crude silver tetrafluoroborate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110165728.XA CN112960678A (en) | 2021-02-06 | 2021-02-06 | Method for removing crystal water and purifying crude silver tetrafluoroborate |
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