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Microemulsion and Oil Soluble Gassing System

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Microemulsion and Oil Soluble Gassing System Europaisches Patentamt (19) European Patent Office Office europeeneen des brevets £P 0 775 681 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) intci.6: C06B 23/00, C06B 47/14 28.05.1997 Bulletin 1997/22 (21) Application number: 96308223.5 (22) Date of filing: 14.11.1996 (84) Designated Contracting States: (72) Inventor: Chattopadhyay, Arun Kumar DE FR GB SE Quebec J4Z 3E6 (CA) (30) Priority: 24.11.1995 CA 2163682 (74) Representative: Ede, Eric Fitzpatricks, (71) Applicant: ICI Canada Inc. 4 West Regent Street North York Ontario M2N 6H2 (CA) Glasgow G2 1 RS, Scotland (GB) (54) Microemulsion and oil soluble gassing system (57) The present invention relates to a process for microemulsions of the present invention provides more preparing an emulsion explosive which has been sensi- complete mixing of the gas precursor with the constitu- tized by the in-situ gassing of a chemical gassing agent, ents of the emulsion explosives. The process thus pro- wherein the gassing agent is contained in a microemul- vides a more controllable reaction for the in-situ, chem- sion. The invention also relates to the microemulsions ical gassing of emulsions, and for the production of utilized in the practise of this process. The use of the chemically gassed emulsion explosives at lower tem- perature. FIGURE Density (g/cc) i 1.3 1.2 1.1 h 1.0 00 CO 30 Time (mins) lO Is- Is- o a. LU Printed by Jouve, 75001 PARIS (FR) EP 0 775 681 A1 Description Field of the Invention 5 This invention relates to an improved process for preparing an emulsion explosive and incorporation of a dispersed gaseous phase within the emulsion. The invention particularly relates to the sensitization of emulsion explosives by chemical gassing using a microemulsion system dispersed in the continuous oil phase of the emulsion. Description of the Related Art 10 Emulsion explosive compositions are well known in the explosives industry. The emulsion explosive compositions now in common use were first disclosed in the U.S. Patent Number 3,447,978 (Bluhm) and comprise as components: (a) a discontinuous aqueous phase comprising discrete droplets of an aqueous solution of inorganic oxygen-releasing salts; (b) a continuous water-immiscible organic phase throughout which the droplets are dispersed; (c) an emulsifier is which forms an emulsion of the droplets of oxidiser salt solution throughout the continuous organic phase; and pref- erably (d) a discontinuous gaseous phase. In some emulsion explosives compositions the discontinuous phase com- prises little or no water and this type of emulsion explosive is often referred to as a eutectic emulsion or melt-in-oil emission. Emulsion compositions are often blended with a solid particulate oxidiser salt which may be coated with an organic 20 fuel to provide a relatively low cost explosive of excellent blasting performance. These types of blends are usually referred to as "doped emulsions". Compositions comprising blends of a water-in-oil emulsion and ammonium nitrate (AN) prills or AN prills coated with fuel oil (ANFO) are described in Australian Patent Application No. 29408/71 (But- terworth) and US Patent Nos. 3161551 (Egly et al), 4111717 (Clay), 4181546 (Clay) and 4357184 (Binet et al). Fur- thermore, United States Patent No. 4775431 (Mullay) describes the combination of a water-in-oil macroemulsions with 25 solid particulate oxidiser salts to provide an explosive composition of high density, that is, of higher density than ANFO. US Patent 4907368 (Mullay & Sohara) describes the combination of microemulsions with solid particulate oxidiser salts to form an explosive composition having a density greater than ANFO wherein the microemulsion system acts to increase the density of the oxidiser salt. It is well known in the art to use a gaseous phase to sensitise emulsion explosives and emulsion blends with AN 30 or ANFO. In preparing these gas-sensitised products it is important to achieve an even distribution of gas bubbles of desired size. The methods currently used to incorporate a gaseous phase into emulsion explosives include in situ gassing using chemical agents such as nitrite salts and the incorporation of closed cell, void material such as microballoons or a mixture of gassing and microspheres or porous materials such as expanded minerals such as perlite. While microbal- 35 loons provide voids of constant volume and can be evenly distributed throughout an emulsion they are relatively ex- pensive to use compared with chemical gassing and their use is limited to plant manufacturing facilities because they are difficult to use in the field. Mechanical mixing methods have also been used to entrain a gas phase into an emulsion, however such methods often do not provide efficient dispersion of the gas and consequently the stability of the gas phase is poor due to 40 coalescence and escape of gas bubbles. Attempts have been made to overcome some of these problems by the use of certain chemical agents to control gas bubble size and stabilize the bubbles. Australian Patent Application No. 25706/88 and Australian Patent No. 578460 (Curtin & Yates) disclose mechanical methods of entraining gas bubbles in emulsions and the use of a chemical agent to provide a stable gaseous phase, even in low viscosity emulsion explosives which are essentially wax free. 45 In situ chemical gassing of emulsions is usually carried out by mixing a chemical agent into the emulsion, which agent decomposes or reacts under the influence of one of the components of the emulsion to form gas bubbles. Suitable chemicals include peroxides such as hydrogen peroxide, nitrite salts such as sodium nitrite, nitrosoamines such as N, N'dinitroso-pentamethylenetetramine, alkali metal borohydrides such as sodium borohydride and bases such as car- bonates including sodium carbonate. so The most preferred chemical gassing agent for emulsions comprising ammonium nitrate is sodium nitrite which under conditions of acid pH reacts with the discontinuous phase of the emulsion to produce nitrogen gas bubbles. The decomposition of sodium nitrite can be described chemically as follows: 55 2 EP 0 775 681 A1 N02" + NHA" = N2 + 2 H20 (1) 2 N02" + 2 H+ = NO + H20 (2) 5 3 N02~ + NH<,+ + 2 H+ = N2 + NO + N02 + 3 H20 (3) 10 The auto decomposition of nitrites into nitrogen oxides is favoured by the relatively higher concentrations of nitrites which are present in conditions of acidic pH. It is important that the gassing agent is mixed with the emulsion in such a way that there is ample opportunity for it to interact with the droplets of oxidiser salt in the discontinuous phase. There must be a large number of locations for micro reaction between the gassing agent and oxidiser salt. The gassing reaction rate may be increased by chemical is accelerators known in the art for accelerating the decomposition of a nitrite gassing agent. Such accelerators are either incorporated in the discontinuous phase of the emulsion during manufacture or added to aqueous nitrite solution which is added to the oxidiser or emulsion. In order for the gassing reaction to occur uniformly it is necessary that the gassing agent be dispersed homoge- nously throughout the emulsion. Poor distribution of the gassing agent will affect the size and distribution of gas bubbles 20 formed in the emulsion explosive and may adversely affect the reaction efficiency and even the reaction pathway may be altered. The ease with which the gassing agent is dispersed in emulsions depends on several factors including the nature of the carrier medium, the viscosity of the emulsion matrix and the devices used for dispersing the gassing agent in the emulsion. Most ungassed or "base" emulsions used for emulsion explosive compositions have a density of about 25 1 .3 to 1 .6 g/cc and this is reduced to between 0.9 and 1.1 g/cc by gassing. Chemical gassing agents of the prior art are usually in the form of aqueous solutions or macroemulsions. The amount of chemical gassing agent used to achieve the aforementioned decrease in density is relatively small and there are inherent difficulties in achieving a homogeneous dispersion of small quantities of gassing agent in comparatively large quantities of emulsion. Regardless of the dis- persion devices or carrier media or physical forms of the gassing agent, current gassing technology is limited in the 30 degree of homogeneity that can be achieved in dispersing the gassing agents into the base emulsion. A further difficulty with present in-situ gassing procedures is that the gassing reaction is temperature sensitive and must presently be conducted at elevated temperatures (typically greater than 40°C) in order to effect gassing at an acceptable reaction rate. 35 Summary of the Invention It has now been found that improved gassing of base emulsions for emulsion explosive manufacture can be pro- vided by use of a gassing agent in the form of a microemulsion which can be dispersed in ultra fine physical form throughout the base emulsion. The present invention therefore provides an emulsion explosive gassing agent com- 40 prising a chemical gassing precursor, wherein said gassing precursor is present in a microemulsion comprising an aqueous solution of a gas precursor in an organic phase. Preferably, the microemulsion gassing agent is a water-in-oil microemulsion of: an aqueous solution of a gas precursor; and organic phase; and at least one microemulsion-forming emulsifying agent. In accordance with the present invention, dispersion of said microemulsion gassing agent in a base emulsion will 45 lead to decomposition, or more generally, reaction of said gas precursor to form gas bubbles in said base emulsion. Accordingly, the present invention provides a process for the manufacture of gassed emulsion explosives, and provides gassed emulsion explosives which have been gassed through the use of the microemulsions of the present invention.
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