Description:DETAILED DESCRIPTION OF THE INVENTION
[0013] Those skilled in the art will be aware that the present disclosure is subject to variations and modifications other than those specifically described. It is to be understood that the present disclosure includes all such variations and modifications. The disclosure also includes all such steps, features, compositions, and compounds referred to or indicated in this specification, individually or collectively, and any and all combinations of any or more of such steps or features.
Definitions
[0014] For convenience, before further description of the present disclosure, certain terms employed in the specification, and examples are delineated here. These definitions should be read in the light of the remainder of the disclosure and understood as by a person of skill in the art. The terms used herein have the meanings recognized and known to those of skill in the art, however, for convenience and completeness, particular terms and their meanings are set forth below.
[0015] The articles “a”, “an” and “the” are used to refer to one or to more than one (i.e., to at least one) of the grammatical object of the article.
[0016] The terms “comprise” and “comprising” are used in the inclusive, open sense, meaning that additional elements may be included. It is not intended to be construed as “consists of only”.
[0017] Throughout this specification, unless the context requires otherwise the word “comprise”, and variations such as “comprises” and “comprising”, will be understood to imply the inclusion of a stated element or step or group of elements or steps but not the exclusion of any other element or step or group of element or steps.
[0018] The term “including” is used to mean “including but not limited to”. “Including” and “including but not limited to” are used interchangeably.
[0019] The term “Fluoroboric acid” is used to mean “Tetrafluoro boric acid”. “Fluoroboric acid” and “Tetrafluoroboric acid” are used interchangeably.
[0020] Ratios, concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, the process is carried out at a temperature in a range of -20 to 50°C should be interpreted to include not only the explicitly recited limits of -20 to 50°C but also to include sub-ranges, such as -15 to 30°C, -19 to 24°C, 40 to 50°C and so forth, as well as individual amounts, including fractional amounts, within the specified ranges, such as -18.5°C, -14.9°C, -10.6°C, -5.6°C, 40°C, 45°C and 48°C.
[0021] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the disclosure, the preferred methods, and materials are now described. All publications mentioned herein are incorporated herein by reference.
[0022] The present disclosure is not to be limited in scope by the specific embodiments described herein, which are intended for the purposes of exemplification only. Functionally equivalent products, compositions, formulations, and methods are clearly within the scope of the disclosure, as described herein.
[0023] As discussed in the background of present disclosure, the tetrafluoroboric acid can be synthesized with traditional methods like reaction of hydrogen fluoride with boric acid. Therefore, over the years via conventional reaction of boric acid or metaborate or boron trioxide with hydrogen fluoride synthesis of these tetrafluoroboric acid solvates thereof has been widely explored. However, drawbacks associated with the known process are the use of excess boric acid, metaboric acid or boron trioxide leading to unreacted impurity which impact quality of product. These work at very high temperature results in a tedious process. However, removal of excess boric acid, metaboric acid or boron trioxide or hydrogen chloride at purification step also end up into an expensive, economically non-viable process. Along with this, these processes also result in the formation of high colour tetrafluoroboric acid and solvate with undesired impurities, which hampers the quality of tetrafluoroboric acid and solvates thereof. Thus, to get the pure tetrafluoroboric acid and solvates thereof an extra purification step is always required for these crude tetrafluoroboric acid and solvates thereof only then these can be used for known application.
[0024] Hence to overcome all of these drawbacks present disclosure discloses an ecofriendly, effective and efficient process for manufacturing tetrafluoroboric acid and solvates thereof, which involves reaction between boron trifluoride or boron trifluoride solvates and hydrogen fluoride. The present disclosure relates to the manufacturing of tetrafluoro boric acid and solvates thereof. The process of present disclosure also involves reaction of cooled hydrogen fluoride with boron trifluoride and suitable solvent. This results in the formation of high-quality tetrafluoro boric acid and solvates. Processing of the reaction mixture for optionally distillation.
[0025] The invented process is conducted at comparatively low temperatures and thus reduces the utility cost, hence making it more competent on the commercial front. Hence the process for preparation of tetrafluoroboric acid and solvates thereof of the present disclosure is an economically viable, highly efficient process for development of high quality tetrafluoroboric acid and solvates thereof.
[0026] Accordingly, the present disclosure provides a process for preparation of a tetrafluoroboric acid and solvates thereof, the process comprising: reaction between boron trifluoride or boron trifluoride solvates with hydrogen fluoride at lower temperature to the manufacturing of tetrafluoro boric acid and solvates thereof. The process of present disclosure also involves reversing of reagent sequence by reaction of cooled hydrogen fluoride with boron trifluoride followed by addition of suitable solvents.
[0027] The present disclosure is not to be limited in scope by the specific embodiments described herein, which are intended for the purposes of exemplification only. Functionally equivalent products, compositions, and methods are clearly within the scope of the disclosure, as described herein.
[0028] In an embodiment of the present disclosure, there is provided a process for preparation of a tetrafluoroboric acid and solvates thereof as disclosed herein, wherein the process is carried out at a temperature in a range of -20°C to 50°C, at an atmospheric pressure to 15 kg/cm2 pressure, and for a period in a range of 2 to 10 hours. In another embodiment, the process is carried out at a temperature in a range of -10°C to 40°C, at an atmospheric pressure to 10 kg/cm2 pressure, and for a period in a range of 3 to 8 hours. In yet another embodiment, the process is carried out at a temperature in a range of 0°C to 30°C, at an atmospheric pressure to 5 Kg/cm2 pressure, and for a period in a range of 4 to 6 hours.
[0029] In an embodiment of the present disclosure, there is provided a process for preparation of tetrafluoroboric acid and solvates thereof as disclosed herein, wherein the obtained tetrafluoroboric acid is optionally distilled out.
[0030] In an embodiment of the present disclosure, there is provided a process for preparation of tetrafluoroboric acid and solvates thereof as disclosed, wherein the tetrafluoroboric acid and solvates thereof has concentration of HBF4 30% to 50%. In another embodiment tetrafluoroboric acid and solvates thereof has concentration of HBF4 50% to 60%. In yet another embodiment, tetrafluoroboric acid and solvates thereof has concentration of HBF4 60% to 75%.
[0031] In an embodiment of the present disclosure, there is provided a process for preparation of a tetrafluoroboric acid and solvates thereof as disclosed herein, wherein the tetrafluoroboric acid and solvates thereof has a yield in a range of 98.0 to 99.0% and the tetrafluoroboric acid and solvates thereof has a purity in a range of 98.0 to 99.0%. In another embodiment, the tetrafluoroboric acid and solvates thereof has a yield in a range of 97.0 to 98.0% and the tetrafluoroboric acid and solvates thereof has a purity in a range of 98.5 to 99.5%. In yet another embodiment, tetrafluoroboric acid and solvates thereof has a yield in a range of 96.0 to 97.0% and the tetrafluoroboric acid and solvates thereof has a purity in a range of 99.5 to 99.9%.
[0032] Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible.
EXAMPLES
[0033] The disclosure will now be illustrated with working examples, which is intended to illustrate the working of disclosure and not intended to take restrictively to imply any limitations on the scope of the present disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this disclosure belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice of the disclosed methods and compositions, the exemplary methods, devices, and materials are described herein. It is to be understood that this disclosure is not limited to particular composition, methods, and experimental conditions described, as such methods and conditions may apply. The present invention will be described in a more detailed manner by way of examples. However, these examples should not be construed as limiting the scope of the present invention.
EXAMPLE 1
Preparation of tetrafluoroboric acid and solvates thereof
[0034] Hydrogen Fluoride (HF) was treated with Boron trifluoride (BF3) for 2 to 6 hours at -20° to 50°C, at atmospheric pressure to 15 Kg/cm2 pressure to produce tetrafluoroboric acid which optionally distilled out under high vacuum. After completion of the reaction, suitable solvent was added to produce tetrafluoroboric acid solvent which optionally distilled out under high vacuum. Purity of product is 98.0% to 99.9% and yield is 96.0% to 99.0%.
EXAMPLE 2
Reverse of reagent sequence
[0035] Boron trifluoride (BF3) solvate was treated with hydrogen fluoride (HF) at -20°C to 50°C and atmospheric pressure to 15kg/cm2 pressure to produce tetrafluoroboric acid solvate which optionally distilled out under high vacuum. Purity of product is 98.0% to 99.9% and yield is 96.0% to 99.0.
ADVANTAGES OF THE PRESENT INVENTION
[0036] The present disclosure provides a process for preparation of a tetrafluoroboric acid and solvates thereof, the process comprising (a) reaction of hydrogen Fluoride (HF) with boron trifluoride (BF3) at -20°C to 50°C and atmospheric process to 15 kg/c2 pressure for 2 to 6 hours to produce tetrafluoroboric acid which optionally distilled out under high vacuum. After completion of reaction, suitable solvent was added to produce tetrafluoroboric acid solvate. Purity of product is 98.0% to 99.9% and yield is 96.0% to 99.0. and b) Boron trifluoride (BF3) solvate was treated with hydrogen fluoride (HF) at -20°C to 50°C to produce tetrafluoroboric acid solvate which optionally distilled out under high vacuum. Purity of product is 98.0% to 99.9% and yield is 96.0% to 99.0. The process of the present disclosure reduces the byproducts formation during reaction and achieves tetrafluoroboric acid and solvates thereof with low color and high purity. The process eliminates steps as required in the conventional approaches, high temperature reaction condition and also avoids excess use of starting materials which increases purity of the product. Hence present disclosure provides a process for high quality economical advantageous tetrafluoro boric acid and solvates thereof under mild reaction conditions. These advantages make this process suitable for a wide range of applications.
, Claims:We Claim:
1. A process for preparation of a tetrafluoroboric acid and solvates thereof comprising the steps of:
(a) treating hydrogen fluoride (HF) with boron trifluoride (BF3) to produce tetrafluoroboric acid;
(b) optionally distilled out tetrafluoroboric acid under high vacuum;
(c) adding of suitable solvents to form tetrafluoroboric acid solvates and
(d) optionally distilled out tetrafluoroboric acid solvates under high vacuum.
2. A process for preparation of a tetrafluoroboric acid and solvates thereof comprising the steps of:
(a) treating boron trifluoride (BF3) solvates with hydrogen fluoride (HF) to produce tetrafluoroboric solvates and
(b) optionally distilled out tetrafluoroboric acid solvates under high vacuum.
3. The process as claimed in claim 1 and claim 2, wherein solvents are selected from water (H2O); diethyl ether ((C2H5)2O); methanol (CH3-OH); ethanol (CH3-CH2-OH); acetonitrile (ACN) and DimethylSulphoxide (DMSO).
4. The process as claimed in claim 1 and claim 2, wherein the reaction temperature is in the range of -20° to 50°C.
5. The process as claimed in claim 1 and claim 2, wherein the reaction pressure is in the range of an atmospheric pressure to 5.0 Kg pressure.
6. The process as claimed in claim 1 and claim 2, wherein the reaction time is in the range of 2.0 to 10.0 hours.
7. The process as claimed in claim 1 and claim 2, wherein the yield of tetrafluoroboric acid and solvates thereof is in the range of 96.0 to 99.0%.
8. The process as claimed in claim 1 and claim 2, wherein the purity of the tetrafluoroboric acid and solvates thereof is in the range of 98.0 to 99.9%.
9. The process as claimed in claim 1 and claim 2, wherein the concentration/Assay of tetrafluoroboric solvate is in the range of 30% to 75% fluoroboric acid concentration.