US 7,740,775 B2Granted

Method for the production of particles

AssigneeGlaxo Group Limited

InventorsMazin Nicola, Neale Gray

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Abstract

A process for preparing particles of a substance comprising contacting a first formulation including a first substance with a first solvent stream and a second solvent stream, thereby causing formation of particles of the first substance, wherein both the first and second solvent streams are in a non-supercritical state, and subjecting the resultant mixture to a separation process which causes separation of the first substance from the first and second solvent streams.

Claims60

Dependent claims

A process for preparing particles of a substance, said process comprising

providing a mixer having a first inlet connected to a first solvent source comprising a first solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a second inlet connected to a second solvent source comprising a second solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a third inlet connected to a source of a first formulation being a solution of the substance in a carrier solvent, and having an outlet connectable to a separation means for separating particles of the first substance from the first and second solvents, and
extracting the carrier solvent from the formulation and precipitating the substance as particles by introducing said first formulation in the form of a stream into said mixer via said third inlet,
introducing said first solvent in the form of a stream into said mixer via said first inlet at a rate such as to contact 1 volume of said formulation with greater than or equal to 1 volume of said first solvent to thereby form a mixture of the first formulation and the first solvent, and subsequently
introducing said second solvent in the form of a stream into said mixer via said second inlet at a rate such as to contact 1 volume of the so-formed mixture of the first formulation and the first solvent with 8-25 volumes of said second solvent, the pressure of the first and second streams of C1-4 hydrofluorocarbon solvent being 1 to 5 bar G above the vapour pressure of the C1-4 hydrofluorocarbon solvent at the operating temperature, the substance being insoluble or only sparingly soluble in the first and second solvent streams, thereby
causing formation of solid particles of the first substance by extraction of the carrier solvent and precipitation, wherein both the first and second solvent streams are in a non-supercritical state, and
subjecting the resultant mixture to a separation process which causes separation of the first substance from the mixture of carrier solvent and first and second solvent streams;
and wherein contact between the first formulation and the first solvent stream is achieved by means of a mixer comprising three concentric tubes, a first of said concentric tubes being connected to the said first inlet for said first solvent, a second of said concentric tubes being connected to the said second inlet for said second solvent, a third of said concentric tubes being connected to the said third inlet for said first formulation, each of said three concentric tubes having an outlet, wherein the first solvent stream is fed through said first of said three concentric tubes, the second solvent stream is fed through said second of said three concentric tubes, and the first formulation is fed through the third of said three concentric tubes, and the outlets of the three concentric tubes are designed to effect contact between the first formulation, the first solvent stream and the second solvent stream.

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A process for preparing particles of a substance, said process comprising

providing a mixer having a first inlet connected to a first solvent source comprising a first solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a second inlet connected to a second solvent source comprising a second solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a third inlet connected to a source of a first formulation being a solution of the substance in a carrier solvent, and having an outlet connectable to a separation means for separating particles of the first substance from the first and second solvents, and
extracting the carrier solvent from the formulation and precipitating the substance as particles by introducing said first formulation in the form of a stream into said mixer via said third inlet,
introducing said first solvent in the form of a stream into said mixer via said first inlet at a rate such as to contact 1 volume of said formulation with greater than or equal to 1 volume of said first solvent to thereby form a mixture of the first formulation and the first solvent, and subsequently
introducing said second solvent in the form of a stream into said mixer via said second inlet at a rate such as to contact 1 volume of the so-formed mixture of the first formulation and the first solvent with 8-25 volumes of said second solvent, the pressure of the first and second streams of C1-4 hydrofluorocarbon solvent being 1 to 5 bar G above the vapour pressure of the C1-4 hydrofluorocarbon solvent at the operating temperature, the substance being insoluble or only sparingly soluble in the first and second solvent streams, thereby
causing formation of solid particles of the first substance by extraction of the carrier solvent and precipitation, wherein both the first and second solvent streams are in a non-supercritical state, and
subjecting the resultant mixture to a separation process which causes separation of the first substance from the mixture of carrier solvent and first and second solvent streams;
and wherein contact between the first formulation and the first solvent stream is achieved by means of a mixer comprising two concentric tubes, a first of said concentric tubes being connected to the said first inlet for said first solvent, a second of said concentric tubes being connected to the said third inlet for said first formulation, each of said two concentric tubes having an outlet, wherein the first solvent stream is fed through said first of said two concentric tubes and the first formulation is fed through the second of said two concentric tubes, and the outlets of the two concentric tubes are designed to effect contact between the first formulation and the first solvent stream.

4 more elements

A process for preparing particles of a substance, said process comprising

providing a mixer having a first inlet connected to a first solvent source comprising a first solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a second inlet connected to a second solvent source comprising a second solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a third inlet connected to a source of a first formulation being a solution of the substance in a carrier solvent, and having an outlet connectable to a separation means for separating particles of the first substance from the first and second solvents, and
extracting the carrier solvent from the formulation and precipitating the substance as particles by introducing said first formulation in the form of a stream into said mixer via said third inlet,
introducing said first solvent in the form of a stream into said mixer via said first inlet at a rate such as to contact 1 volume of said formulation with greater than or equal to 1 volume of said first solvent to thereby form a mixture of the first formulation and the first solvent, and subsequently
introducing said second solvent in the form of a stream into said mixer via said second inlet at a rate such as to contact 1 volume of the so-formed mixture of the first formulation and the first solvent with 8-25 volumes of said second solvent, the pressure of the first and second streams of C1-4 hydrofluorocarbon solvent being 1 to 5 bar G above the vapour pressure of the C1-4 hydrofluorocarbon solvent at the operating temperature, the substance being insoluble or only sparingly soluble in the first and second solvent streams, thereby
causing formation of solid particles of the first substance by extraction of the carrier solvent and precipitation, wherein both the first and second solvent streams are in a non-supercritical state, and
subjecting the resultant mixture to a separation process which causes separation of the first substance from the mixture of carrier solvent and first and second solvent streams wherein the first and second inlets introduce the respective streams of first and second solvent into the mixer in opposite flow directions so that the first and second solvent streams contact each other in a head to head relationship.

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Dependencies are inferred from the claim text.

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Abstract

A process for preparing particles of a substance, said process comprising

providing a mixer having a first inlet connected to a first solvent source comprising a first solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a second inlet connected to a second solvent source comprising a second solvent being a C1-4 hydrofluorocarbon with a boiling point less than 20° C. and more than −90° C., having a third inlet connected to a source of a first formulation being a solution of the substance in a carrier solvent, and having an outlet connectable to a separation means for separating particles of the first substance from the first and second solvents, and
extracting the carrier solvent from the formulation and precipitating the substance as particles by introducing said first formulation in the form of a stream into said mixer via said third inlet,
introducing said first solvent in the form of a stream into said mixer via said first inlet at a rate such as to contact 1 volume of said formulation with greater than or equal to 1 volume of said first solvent to thereby form a mixture of the first formulation and the first solvent, and subsequently
introducing said second solvent in the form of a stream into said mixer via said second inlet at a rate such as to contact 1 volume of the so-formed mixture of the first formulation and the first solvent with 8-25 volumes of said second solvent, the pressure of the first and second streams of C1-4 hydrofluorocarbon solvent being 1 to 5 bar G above the vapour pressure of the C1-4 hydrofluorocarbon solvent at the operating temperature, the substance being insoluble or only sparingly soluble in the first and second solvent streams, thereby
causing formation of solid particles of the first substance by extraction of the carrier solvent and precipitation, wherein both the first and second solvent streams are in a non-supercritical state, and
subjecting the resultant mixture to a separation process which causes separation of the first substance from the mixture of carrier solvent and first and second solvent streams;
and wherein contact between the first formulation and the first solvent stream is achieved by means of a mixer comprising three concentric tubes, a first of said concentric tubes being connected to the said first inlet for said first solvent, a second of said concentric tubes being connected to the said second inlet for said second solvent, a third of said concentric tubes being connected to the said third inlet for said first formulation, each of said three concentric tubes having an outlet, wherein the first solvent stream is fed through said first of said three concentric tubes, the second solvent stream is fed through said second of said three concentric tubes, and the first formulation is fed through the third of said three concentric tubes, and the outlets of the three concentric tubes are designed to effect contact between the first formulation, the first solvent stream and the second solvent stream.

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