The actual concentration of bromine in the product zinc bromide stream will depend on the temperature, zinc bromide concentration, etc. Preferably the resulting product is collected at vessel top 34. 1 is a schematic of a method of batch production of zinc bromide according to the present invention. The reaction solvent feed can comprise halide ions to improve solubility of the bromine in the reaction solvent. Concentration can occur by evaporation of the solution. The method of claim 12 wherein the reaction vessel comprises a single stage reactor. Assignors: TETRA PRODUCTION TESTING SERVICES, LLC, TETRA TECHNOLOGIES, INC. RELEASE BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). 4. If I use this method i would end up using 2400g of ZBr2 to make the 1 liter solution, that seems like a lot to me. The metal of the metal halide salt can be selected from the group consisting of alkali metals, alkaline earth metals, transition metals and combinations thereof. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). The apparatus from Example 3 was modified to allow the recycle zinc bromide solution to be drawn from between lower and upper column sections as shown in FIG. A method for making zinc bromide from metallic zinc and bromine comprising contacting zinc with bromine dissolved in a reaction solvent containing a metal halide salt. The method of claim 1 wherein the temperature of the method is controlled by continuously adding bromine to the reaction solvent at a rate that maintains the reaction temperature below the boiling point of bromine. [1], 3 (1), 17-33 (1940). Bromine has a noxious, acrid odor, and the maximum health and safety exposure limit is currently 1 ppm in the air. The product solution was 30.8% zinc bromide and 0.01% bromine. The resulting zinc bromide which dissolves in the reaction solvent can be drawn off in solution in a batch mode or recycled along with the reaction solvent and bromine. ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:TETRA TECHNOLOGIES, INC.;REEL/FRAME:011159/0741, Owner name: The metallic zinc 38 is contacted with the bromine/reaction solvent solution to form zinc bromide. 3. In a preferred method as depicted in FIG. The residence time of the bromine solution in contact with the zinc metal is preferably long enough so that substantially complete reaction of the bromine with the zinc occurs, leaving the reaction solvent effluent eventually free of elemental bromine and enriched in zinc bromide. The method of claim 1 comprising the further step of concentrating the zinc bromide solution. At least a proportion of the zinc bromide solution resulting from contacting the zinc shot with the bromine/reaction solution is drawn from the lower section 46 and recycled back to the mixer 50. Heat from the reaction causes water to evaporate as steam. The apparatus consisted of a glass chromatography column, feed flask, and chemical metering pump as shown in FIG. Assignors: SYMENS, RAYMOND D., HANLON, DAVID J., DUNAWAY, WEYMAN H., MCKENNIS, JEFFREY S., HOWARD, LYLE H. Assigned to TETRA INVESTMENT HOLDING CO., INC. NUNC PRO TUNC ASSIGNMENT (SEE DOCUMENT FOR DETAILS). More preferably, the bromine is dissolved in the presence of an aqueous solution of a halide ion. The method of claim 1 wherein the bromine is added continuously to the reaction solvent. Any remaining product stream enters the upper section 48 of the reaction vessel 40 for continued reaction with the zinc shot and the resulting product stream can be drawn off from the top of the vessel top 44. The lower section was 12-inch tall and the upper section was 24-inch tall. No. The mixing vessel was fed 3.9 g/min bromine and 2.4 g/min water and allowed to mix with recycled zinc bromide solution containing 59.5% zinc bromide. A method for making zinc bromide comprising: (a) dissolving bromine in an aqueous reaction solvent comprising a metal halide salt; and. The method of claim 1 wherein the halide of the metal halide salt is selected from the group consisting of chloride and bromide. The solution of bromine, water and zinc bromide was pumped from the mixing vessel, through a heat exchanger and into the bottom of the column. The specific feed solvent concentration of bromine will depend on the solubility of bromine in the zinc bromide brine, the residence time of the solvent in contact with the zinc metal, temperature, reaction kinetics and the like. Somewhere I am missing the calculation concept that will allow me to find the mass of zinc bromide (solids) to add to 1 liter of water to get the specified specific gravity? In the method of this invention, zinc bromide is produced directly from its elements. Preparing a solution of zinc bromide with a specific gravity of 2.40. The recycle rate was approximately 232 ml/min. Feed samples were prepared by metering bromine and water into the mixing vessel. SECURITY INTEREST;ASSIGNORS:TETRA TECHNOLOGIES, INC.;TETRA PRODUCTION TESTING SERVICES, LLC;REEL/FRAME:047526/0436, Free format text: However, a preferred concentration at the start of the reaction is within a range from about 0.001 weight percent base metal halide up to saturation. I'm pretty sure that's how you should be looking at this. Preferably, the reaction solvent is aqueous. In one aspect of this invention, the zinc bromide solution is concentrated by evaporation. The column used for this experiment was a commercially available 12-inch tall column having an inside diameter of 1 inch. I need to make a zinc bromide solution with a specific gravity of 2.40, how can I do this? The reaction of metallic zinc with halides to produce a zinc halide was reported over 150 years ago. The method of claim 8 wherein the zinc bromide solution is concentrated by evaporation. MERGER;ASSIGNOR:TETRA-CHLOR, INC.;REEL/FRAME:011149/0327, Owner name: Production of Zinc Bromide Solution from Zinc Metal, Bromine and Water. According to the MSDS the density of Zinc Bromide is 4.22g/ml and this is where I am getting turned around I need to make a solution of Zinc Bromide that has a specific gravity of 2.4. TETRA TECHNOLOGIES, INC., TEXAS, Free format text: The column was filled with 3-5 mm zinc shot from Fisher Scientific. Application filed by Tetra Technologies Inc. The product is essentially color free. Bromine vapor pressure is very difficult to measure, but by extrapolation from this published data, we believe that bromine vapor pressure is also reduced by lower bromine concentration. The solution of bromine, water and zinc bromide was pumped from the feed flask into the bottom of the column. A. Raynaud, Bull. The process of preparing metal bromides from free metals and bromine has been reported in patent literature. Alternatively, bromine can be dissolved in the reaction solvent fed into the reaction vessel. The resulting solution was 58.7% zinc bromide and 0.9% bromine. Chim. 1. The preferred metal halide salt is selected from the group consisting of sodium, potassium, calcium, zinc and a combination thereof. The reaction solvent 56 containing the dissolved bromine is fed into the reaction vessel 30 or column containing metallic zinc 38, zinc shot for example. Soc. Alternatively, zinc bromide can be concentrated by increasing the percent of zinc bromide in solution by recycling at least a portion of the zinc bromide product stream back to contact with the metallic zinc. In one embodiment, zinc shot is suspended in a reaction solvent and bromine is added directly to the reaction solvent. Therefore, it is reasonable to include that products from this invention containing lower concentrations of bromine should also have lower bromine odor. 3,723,075 to Stevenson et al., discloses that aluminum tribromide is made by reacting metallic aluminum with bromine in a stirred liquid reaction medium consisting essentially of molten aluminum tribromide at temperatures of 100° C. to 140° C. None of the references teach or suggest a method for manufacturing zinc bromide from metallic zinc and bromine solution on a large scale, commercial basis. The top of the column was fitted with an adapter that allowed gas and liquid to leave the column separately.


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