MICROPARTICLES AND METHOD OF MAKING MICROPARTICLES

• US 20120148636A1
• Filed: 06/24/2010
• Published: 06/14/2012
• Est. Priority Date: 06/24/2009
• Status: Active Grant

• Current Assignee: Bell Flavors & Fragrances Duft Und Aroma GmbH
• Original Assignee: Bell Flavors & Fragrances Duft Und Aroma GmbH
• Inventors: Berrido, Colin, Huppert, Hans-Jurgen, Rabke, Peter
• Granted Patent: US 9,493,728 B2
• Time in Patent Office: Days
• US Class Current: 424/400
• CPC Class Codes: A61K 2800/56 Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
• CPC Class Codes: A61K 2800/652 The particulate/core comprising organic material
• CPC Class Codes: A61K 8/0245 Specific shapes or structures not provided for by any of the groups of A61K8/0241
• CPC Class Codes: A61K 8/342 Alcohols having more than seven atoms in an unbroken chain
• CPC Class Codes: A61Q 19/00 Preparations for care of the skin
• CPC Class Codes: C11D 17/0013 Liquid compositions with insoluble particles in suspension C11D17/0021, C11D17/0026, C11D17/003 take precedence
• CPC Class Codes: C11D 3/18 Hydrocarbons C11D3/164 takes precedence
• CPC Class Codes: C11D 3/201 linear
• CPC Class Codes: C11D 3/2013 fatty or with at least 8 carbon atoms in the alkyl chain
• CPC Class Codes: C11D 3/3719 Polyamides or polyimides
• CPC Class Codes: C11D 3/3765 in liquid compositions
• CPC Class Codes: C11D 3/384 Animal products
• CPC Class Codes: C11D 3/505 encapsulated or adsorbed on a carrier, e.g. zeolite or clay

Abstract

A process for producing micronized dispersed micro-particles and to micro-particles produced by this process.

Claims

1-84. -84. (canceled)

85. A process of preparing a composition comprising a plurality of micro-particles and a dispersion liquid in which said micro-particles are dispersed comprising the steps of:

providing a high energy micro-particle producing machine comprising a micro-particle producing assembly;

providing a combination of a dispersion liquid, an active and a wax or wax like material at such a temperature that the active and the wax or wax-like components of the combination are melted;

passing said combination into said micro-particle producing assembly of said high energy micro-particle producing machine whilst said micro-particle producing assembly is operating at such a temperature that said active and said wax or wax-like components of the combination are kept melted then while said micro-particle producing assembly is kept operating producing a composition comprising a plurality of micro-particles dispersed in said dispersion liquid by cooling said combination to a temperature below the solidification temperature of each of said micro-particles before each said micro-particle leaves said micro-particle producing assembly, each said micro-particle comprising a wax or wax-like dispersion matrix with said active dispersed therein.

86. A process according to claim 85, wherein said high energy micro-particle producing machine further comprises a feeding assembly and means for providing fluid flow communication between said feeding assembly and said micro-particle producing assembly said high energy micro-particle producing machine further comprising means for opening and closing said fluid flow between said feeding assembly and said micro-particle producing assembly.

87. A process according to claim 86, wherein said combination of said dispersion liquid said active and said wax or wax like material are provided in said feeding assembly at such a temperature that the active and the wax or wax like components are melted with fluid flow between said feeding assembly and said micro-particle producing assembly closed and then said fluid flow is opened.

88. A process according to claim 86, wherein said feeding assembly comprises heating means for melting or keeping melted said active and said wax or wax-like components of said combination.

89. A process according to claim 86, wherein said means for providing fluid flow communication further comprises insulating means for keeping said active and said wax or wax-like components of said combination melted during flow.

90. A process according to claim 85, comprising the additional steps of recycling said composition comprising said plurality of micro-particles dispersed in said dispersion liquid through the micro-particle producing assembly one or more times whilst cooling is continued such that said composition comprises further micro-particles dispersed in said dispersion liquid.

91. A process according to claim 85, wherein said composition is diluted with a dilution liquid after said composition has left said high energy micro-particle producing machine for the final time.

92. A process according to claim 91, wherein said dilution liquid is selected from propylene glycol, a blend of surfactants suitable for use as a laundry detergent base, a blend of surfactants suitable for use as a fabric conditioner, glycerol, water and a combination of water and a surface tension lowering agent.

93. A process according to claim 92, wherein said dilution liquid is sufficiently cold further to reduce the temperature of said composition.

94. A process according to claim 85, wherein said composition is further cooled by a cooled heat exchanger after said composition has left said high energy micro-particle producing machine for the final time.

95. A process according to claim 90, wherein said a high energy micro-particle producing machine is provided with a temperature regulating assembly for controlling the temperature of said combination as it passes through said micro-particle producing assembly.

96. A process according to claim 95, wherein said temperature regulating assembly is operated during a first step of operation to hold the temperature of said combination at such a first temperature that said active and said wax or wax-like components of the combination are kept melted when said combination is passed into said micro-particle producing assembly and then is operated during a second step of operation to hold the temperature of said combination at such a second temperature that said plurality of micro-particles are produced by cooling said combination to a temperature below the solidification temperature of each of said micro-particles before each said micro-particle leaves said micro-particle producing assembly.

97. A process according to claim 85, wherein said temperature regulating assembly is a cooling jacket which provides said cooling of said combination to a temperature below the solidification temperature of each of said micro-particles before each said micro-particle leaves said micro-particle producing assembly.

98. A process according to claim 85, wherein said cooling is provided by introducing additional dispersion liquid into said micro-particle producing assembly at a sufficiently low temperature to cool said combination to a said temperature below said solidification temperature of each of said micro-particles.

99. A process according to claim 85, wherein said high energy micro-particle producing machine is a Sonic mill equipped with a stopcock downstream from its feeding funnel.

100. A process according to claim 99, wherein said feeding funnel is equipped with a immersion heater and a stirrer.

101. A process according to claim 85, wherein said high energy micro-particle producing machine is a colloid mill having sufficiently high shearing power to produce said micro-particles each having up to 80% by weight of said active dispersed in said wax or wax-like dispersion matrix.

102. A process according to claim 85, wherein said dispersion liquid is selected from propylene glycol, a blend of surfactants suitable for use as a laundry detergent base, a blend of surfactants suitable for use as a fabric conditioner and glycerol.

103. A process according to claim 102, wherein said process is an in-line process where said produced composition comprising a plurality of micro-particles dispersed in said dispersion liquid is fed into a line of a further process.

104. A process according to claim 85, wherein said dispersion liquid comprises a surface tension lowering agent.

105. A process according to claim 104, wherein said process is a batch process wherein said produced composition comprising a plurality of micro-particles dispersed in said dispersion liquid is collected batch wise as a final product of said process, or an in-line process.

106. A process according to claim 85, each said micro-particle comprising from 20 to 80 weight percent of said active.

107. A process according to claim 85, comprising a further step of collecting said plurality of micro-particles dispersed in said dispersion liquid as a product of the process.

108. A process according to claim 85, where the active is selected from botanical extracts including essential oils, other perfumes and mixture thereof.

109. A process according to claim 85, where each of the wax or wax-like material and the dispersion matrix of the micro-particle is a C22 fatty alcohol.

110. A process according to claim 85, wherein said high energy micro-particle producing machine comprising said micro-particle producing assembly is a high energy rotor-stator machine comprising a rotor-stator assembly.

111. A process according to claim 85, wherein said micro-particle producing assembly comprises an orifice, a means for forcing said combination through said orifice and a surface downstream from said orifice whereby said combination is forced through said orifice towards said surface at such a force that said combination is accelerated to a velocity of at least 300 ft/sec before striking said surface.

112. A process according to claim 111, wherein said means for forcing said combination through said orifice is a pump.

113. A process according to claim 111, wherein said surface can handle pressures of up to 5000 psi.

114. A process according to claim 85, wherein said high energy micro-particle producing machine comprises a rotating mixing portion and a stationary surface surrounding said rotating mixing portion whereby said rotating mixing portion forces said combination towards said stationary surface with such a force that said combination is accelerated to a velocity of at least 300 ft/sec before striking said surface.

115. A composition comprising a plurality of the micro-particles and a dispersion liquid in which said micro-particles are dispersed, each said micro-particle comprising a wax or wax-like dispersion matrix with an active dispersed therein, at least a majority of said micro-particles having a particle size of from 0.1 to 20 micrometers, the wax of said wax or wax like dispersion matrix being a solid at a temperature of 21°

C., and wherein said plurality of micro-particles dispersed in said dispersion liquid are present in said dispersion liquid in an amount of above 20 weight percent.

116. A composition according to claim 115, wherein said plurality of micro-particles are present in an amount of 21 to 60 weight percent.

117. A composition according to claim 115, wherein the micro-particles has a melting point of from 38°

C. to 150°

C.

118. A composition according to claim 115, wherein each said micro-particles comprises up to 80 weight percent of said active.

119. A composition according to claim 115, wherein each said micro-particles comprises from 20 to 80 weight percent of said active.

120. A composition according to claim 115, wherein the wax or wax-like material of the dispersion matrix is a fatty alcohol wax like material or a mixture of said fatty alcohol wax like materials with fatty acid(s) and/or fatty alcohol ethoxylate and/or polyethylene glycol and wherein each said fatty alcohol(s) and said fatty acid(s) have 16-2 carbon atoms, wherein said fatty alcohol ethoxylate has 10-29 carbon atoms, with there being present 5-100 moles of ethylene oxide in each case, and wherein said polyethylene glycol has a molecular weight of 10-30,000 g per mole.

121. A composition according to claim 115, wherein said dispersion liquid is selected from propylene glycol, a blend of surfactants suitable for use as a laundry detergent base, a blend of surfactants suitable for use as a fabric conditioner, glycerol, liquid paraffin oil dispersing agent, and liquid methyl silicone dispersing agent.

122. A composition according to claim 115, wherein said dispersion liquid comprises a blend of water and a surface tension lowering agent capable of lowering the surface tension of the water to 30 dynes/cm or less.