Patent GB-983856-A (GB)
Title: Novel chloroisocyanurate compounds and process for preparing same
IPC: C11D3/395
Filed: 1961-06-14
Abstract: (Mono-trichloro) (mono-potassium dichloro) di - isocyanurate, [(mono - trichloro)tetra-(mono - potassium dichloro)]penta - isocyanurate, i.e. <FORM:0983856/C1/1> <FORM:0983856/C1/2> or mixtures thereof. The two isocyamates or a mixture may be prepared by reacting at 5-50 DEG C. mono-potassium dichloroiso-cyanurate, e.g. 5-12% in H2O, and trichloroisocyanuric acid, e.g. 15-36%, in a liquid, e.g. organic solvent such as acetone, methyl or ethyl alcohol, or an aqueous slurry containing 15-60 parts acid and 40-85 parts H2O. The molecular ratio of the potassium compound to acid may be 1.15-8 : 1 depending on the product desired. The trichloroisocyanuric acid may be prepared in situ. In an example, an aqueous slurry of the pentaisocyanurate was placed in a chlorination vessel comprising a jacketed cylindrical glass container with 3 equidistant vertical baffles, agitated with a propeller A 0.14 mol. excess of aq. KOH was mixed with cyanuric acid to form the tripotassium cyanurate which was filtered, cooled to 10 DEG  C. and then continuously fed via a tube into the bottom of the container while gaseous or liquid Cl2 was fed at 0-50 DEG C. at a rate to give a pH of 2.1-6.0; a portion of the aqueous slurry was continuously removed via a tube at the top of the vessel and the slurry was filtered. The trichloroisocyanuric acid may also be formed in situ by reacting at 5-50 DEG  C. an aqueous solution, e.g. 5-9%, of mono-potassium dichloroisocyanurate and sufficient, e.g. 5-15%, ag. HCl to give a pH of 4.6-5.0 and filtering the precipitate. The processes may be batch or continuous and the isocyanurates may be isolated from the slurries by filtration or centrifuging and may be washed with H2O before drying or used wet.  A composition for use as an oxidizer or abrasive or detergent may contain an organic, e.g. 0.05-25% and/or inorganic compound, e.g. 50-99% (which is inert with respect to the isocyanurate) and 0.05-98% or, e.g. 0.05-50% of the pentadi-isocyanurates or mixtures thereof.  The inorganic compound may include for abrasive compositions dicalcium orthophosphate, CaCO3, CaSO4, TiO2, SiO2, talc and felspar and 0.05-20 isocyanurate. The detergent compositions may contain 1-10% isocyanurate.  The inorganic compound which may be water-soluble or insoluble may be alkaline or neutral, e.g. alkali metal detergent builder salt, alkali and/or alkaline earth metals such as Na, K, Li, Ca, Ba, or Al, Fe and Ti phosphates, silicates, carbonates, aluminates, chlorides, sulphates, and oxides; the phosphates may be orthophosphates such as di- and tri-sodium orthophosphate, pyrophosphates such as tetra sodium pyrophosphate, polyphosphates such as sodium tripolyphosphate, metaphosphates such as sodium trimeta- and hexameta-phosphates; meta-, ortho-, di- and tetra-silicates, e.g. of Na, K, Li and Ca. The organic compound may be a surfactant, e.g. anionic such as sodium alkyl (branched chain with 10-16 C atoms) benzene sulphonate, or sulphated or sulphonated alkyl, aryl and alkylaryl hydrocarbons, non-ionic or cationic; or may be a perfume or odour masking agent, e.g. essential oils, sequestering or chelating agents, e.g. metal salts of ethylene-diamine tetra-acetic acid, dyes and colouring agents, stain, corrosion or tarnish inhibitors.  Some of the groups of organic compounds are defined by references to literature.ALSO:An abrasive or detergent composition comprises 0.05-98% of (mono-trichloro)(mono-potassium dichloro)di-isocyanurate, [(mono-trichloro) tetra - (mono - potassium dichloro)] penta-iso-cyanurate, i.e. <FORM:0983856/C4-C5/1> or mixtures thereof, an organic, e.g. 0.05-25%, and/or inorganic, e.g. 50-99%, compounds. The composition may contain detergent builder salts, e.g. alkali and/or alkaline earth metal and aluminium, iron and titanium phosphates, silicates, carbonates, aluminates, sulphates, chlorides, polyphosphates, or abrasives, e.g. dicalcium orthophosphate, calcium carbonate or sulphate titanium dioxide, silica, talc and feldspar. The detergents may also contain anionic surfactants, e.g. sulphated and sulphonated alkyl, aryl and alkyl-aryl hydrocarbons, and especially sodium dodecyl-benzene sulphonate, and non-ionic surfactants such as the condensate of 9 molar proportions of ethylene oxide with oxotridecanol.  An example of a scouring powder was 90.0% silica, 5% sodium tripoly phosphate, 2.5% soda ash, 2.2 sodium lauryl sulphate and 0.3% of the isocyanurate, and of a dish-washing composition was 45% sodium tripolyphosphate, 2.3% sodium sulphate, 2.3% sodium meta-silicate, 8% soda ash and 1% of the iso-cyanurate.ALSO:A disinfecting sanitizing or sterilizing composition comprises 0,05-98% of (mono-trichloro) (mono-potassium dichloro) di-isocyanurate, [(mono - trichloro) tetra - (mono - potassium dichloro)] penta - isocyanurate, i.e. <FORM:0983856/A5-A6/1> or mixtures thereof, an organic, e.g. 0,05-25%, and/or inorganic compound, e.g. 50-99% (which is inert with respect to the isocyanurate).  The inorganic compound, which may be water soluble or insoluble, may be alkaline or neutral, e.g. alkali and/or alkaline earth metals such as Na, K, Li, Ca, Ba, or Al, Fe and Ti, phosphates, silicates, carbonates, aluminates, chlorides, sulphates and oxides; the phosphates may be orthosuch as di- and tri-sodium orthophosphate, pyrophosphates such as tetra-sodium pyrophosphate, polyphosphates such as sodium tri-polyphosphates, metaphosphates such as sodium trimeta- and hexameta-phosphates; meta-, ortho-, di- and tetra-silicates, e.g. of Na, K, Li and Ca. The organic compound may be a surfactant, e.g. anionic such as sodium alkyl (branched chain with 10-16 C atoms) benzene sulphonate, or sulphated or sulphonated alkyl, aryl and alkyl-aryl hydrocarbons, non-ionic or cationic; or may be a perfume or odour masking agent, e.g. essential oils, sequestering of chelating agents, e.g. metal salts of ethylenediamine tetra-acetic acid, dyes and colouring agents, stain, corrosion or tarnish inhibitors.ALSO:A bleaching composition comprises 0.05-98%, preferably 5-20%, of (mono-trichloro) (mono-potassium dichloro) di-isocyanurate, [(mono-trichloro) tetra-(mono-potassium dichloro)] pentaiso-cyanurate i.e. <FORM:0983856/D1-D2/1> n is 1 or 4 or mixtures thereof, an organic, e.g. 0.05-25%, and/or inorganic compound, e.g. 50-99% (which is inert with respect to the isocyanurate).  The inorganic compound, which may be water soluble or insoluble, may be alkaline or neutral, e.g. alkali and/or alkaline earth metals such as Na, K, Li, Ca, Ba, or Al, Fe and Ti, phosphates, silicates, carbonates, aluminates, chlorides, sulphates and oxides; the phosphates may be ortho-such as di-and tri-sodium orthophosphate, pyrophosphates such as tetrasodium pyrophosphate, polyphosphates such as sodium tri-polyphosphites, metaphosphates such as sodium trimeta- and hexametaphosphates; Meta-, ortho-, di- and tetra-silicates, e.g. of Na, K, Li and Ca. The organic compound may be a surfactant, e.g. anionic such as sodium alkyl (branched chain with 10-16 C atoms) benzene sulphonates, or sulphated or sulphonated alkyl, aryl and alkyl-aryl hydrocarbons, nonionic or cationic; or may be a perfume or odour masking agent, e.g. essential oils, sequestering or chelating agents, e.g. metal salts of ethylenediamine tetra-acetic acid, dyes and colouring agents, stain, corrosion or tarnish inhibitors.  Some of these groups of organic compound are defined by references to literature.