Патент USA US2403767код для вставки
Patented July 9, 1946 » - 2,403,767 UNITED ~ STATES PATENT ‘ ' omen“ " 2,403,767, REsINA'rn 7 Harold M.'Spurlin, Marshallton, Del., assignor to V I I ' ' - Hercules Powder Company, Wilmington, Del., a I’ corporation of Delaware No Drawing. Application August 1.6, 1943, v1 1 Serial No. 498,876 12 Claims. 1 (01. 260-100) . This invention relates to a new composition of , .2, and eth'oxide are both quit e matter and a method‘ for its production. More ‘ ‘ _ insoluble in most sol- I vents and, therefore, di?‘icult to workwith. particularly, it is concerned with; a new resin _ The reactionmay be'carried out in the presence compound and witha method for its production. In accordance with this invention, it has been found that aluminum alkoxide ,diresinates' may or absence of an anhydrous solvent which'does not react with the product. Hence, in place of Varsol and butanol shown in the examples, xyé lene, hexane, diisopropyl ether, carbon tetrachlo be prepared, free of excess resin acids and im purities, by reacting aluminum trialkoxide with ride, etc., may be used. If it is desired to. make use of a solution of aluminum alkoxide diresinate, 10 a-suitable solvent would be, for example,_a high% er. alcohol, such .as isopropyl, butyl, ,amyl, and vent which does not react with the product. If‘ the like, or a hydrocarbon solvent, such asxy rosin in the proportion of 1 mol- of aluminum tri alkoxide to 2 mols of rosin. The reaction may-be carried out in the presence of an anhydrous sol lene, hexane,‘ isopropyl ether, carbon, tetrachlol desired, the aluminum monoalkoxide diresinate , may be used in solution or the alcohol set free may be distilled o?. ‘ , v a . . . Having thus indicated the general nature and purpose of the invention,’ the following examples :15 are given to illustrate the preparation of'the new ‘ resin compound. In the examples, the term "parts” represents weight units unless otherwise indicated. ' , Example 1 i - ride, etc. ' When; an alcoholis used fora solvent, the alkoxide groupof the ‘aluminum alkoxide- di; resinate will be partially exchanged for the alkoxr ide'group corresponding to the alcohol‘ solvent. Since ‘the alkoxide ‘ group of the‘ aluminum alkoxide ‘diresinate is readily hydrolyzed by wa .20 ter, anhydrous conditions must be usedvin the preparation of the diresinates and dry solvents , r mustbeused. _ , l‘ 1‘ The term “rosin” a's de?ned herein and inlthe 302 parts oi’vrosin crystals and 102 parts of claims, and which may be used in the preparation of aluminum alkoxide diresinates, includes any wood or gum rosin, rosin crystals, oleoresin, rosin acids obtainable therefrom, such as abietic acid, pimaric acid, sapinic acid, etc., as well as mix addition of 3150 parts of dry isopropyl alcohol, 30 tures thereof. In addition, it includes the modi ?ed rosins, such as hydrogenated rosin, heat-v the aluminum isopropoxide diresinate precipi~ treated rosin, polymerized rosin, and the like. tated as a resin which was completely soluble in In carrying out the process described in the xylene. ' invention, an aluminum trialkoxide, such as, for Example 2 35 example, aluminum triisopropoxide, and rosin are reacted in the proportion of 1 mol of aluminum 85 parts of rosin crystals were dissolved in 200 parts of dry butanol containing 29 parts of alu trialkoxide to 2' mols of rosin and, if desired, minum triisopropoxide. A clear solution resulted the alcohol set free may be distilled off. The re and dilution with 1200 parts of butanol caused action may be carried out in the presence or no precipitate of aluminum dialkoxide mono 40 absence of an anhydrous solvent. If the alcohol resinate which is insoluble in butanol. has been driven o?, a higher alcoh'ol, such as dry isopropyl alcohol, may be added to the residue As shown in the examples, the aluminum al and aluminum alkoxide diresinate will be precip koxide diresinate is prepared by'reacting alu itated as a resin. The product can be easily re minum trialkoxide and rosin in the proportion of 1 mol of aluminum trialkoxide to 2 mols of 45 covered by ?ltration. Any other suitable meth od of recovering the aluminum alkoxide diresi rosin, either with or, without distilling o? the nate may be used. » alcohol set free. While aluminum triisopropoxide aluminum triisopropoxide in Varso (astraight 25 run petroleum fraction boiling between 300°—400°. F.) were heated to 150° C. to distill oif 60 parts of isopropyl alcohol. The residue was a solution of aluminum isopropoxide diresinate in Varsol. On has been used as the aluminum trialkoxide, other If a solution of aluminum alkoxide diresinate is desired, the rosin and aluminum trialkoxide trialkoxides of aluminum, such‘ as methoxide, ethoxide, propoxide, butoxide, etc., may be used. 50 may be dissolved in a higher alcoh‘ol, such as butanol, or in any hydrocarbon, ether, or chloé , However, it is preferable to use the triisopropox , rinated solvent, and a clear solution of aluminum ide or tributoxide, since aluminum triisopropox ' alkoxide diresinate results. ide and tributoxide are more readily prepared, the triisopropoxide being the lower boiling and, there There is thus provided by this invention ‘a nevi7 fore, the more readily puri?ed, and the methoxide 55 composition of matter, aluminum alkoxide d1 2,403,767 3 resinate, free of excess acid ‘and impurities, and a method for preparing it. This diresinate is a de?nite compound which is insoluble in isopropyl alcohol in contrast with the dialkoxide monoresinate and triresinate, both of whichmare quite. soluble in this alcohol. What I claim: and‘ desire to protect by Letters Patent is: 1. As a product, aluminum isopropoxide di resinate. 2. The method of producing aluminum iso propoxide diresinate which comprises reacting under anhydrous conditions aluminum triiso propoxide and rosin in the proportionof 1 mol of aluminum triisopropoxide to 2 mols of rosin_ 3. The method of producing aluminum iso— propoxide diresinate which comprises reacting; under anhydrous conditions aluminum triiso propoxide and rosin crystals in the proportion of' 4 aluminum triisopropoxide and polymerized rosin in the proportion of 1 mol of aluminum triiso propoxide to 2 mols of polymerized rosin in the presence of an anhydrous solvent. 8. The method of producing aluminum iso propoxide diresinate which comprises reacting aluminum triisopropoxide and polymerized rosin in the proportion of 1 mol of aluminum triiso propoxide to 2 mols of polymerized rosin in the presence of an anhydrous solvent, distilling off the alcohol set ‘free, and recovering aluminum iso propoxide diresinate from the solution. 9; The method of producing ‘aluminum iso propoxide diresinate which comprises reacting under anhydrous conditions aluminum triiso propoxideand hydrogenated rosin in the propor tion. of 1 mol of aluminum triisopropoxide to.2 mols oihydrogenated rosin. 10. The method of producing aluminum iso 1 mol of aluminum triisopropoxide to 2 mols oi 20 propoxide diresinate which comprises reacting rosin crystals. ' aluminum triisopropcxide and'hyd'rogenated rosin in the proportion of I- mol of‘ aluminum triiso 4. The method‘ of producing aluminum iso propoxide to 2‘ mols: of hydrogenatedfrosinlin the propoxi'de- diresinate which comprises- reacting presence of an anhydrous solvent; aluminum triisopropoxide and rosin crystals in 11‘. The method‘ of producing aluminum iso the proportion of 1‘ mol of" aluminum, triiso 25 propoxide diresinate which comprises reacting propoxide to- 2 mols of'rosinl crystals in the'pres ence of an anhydrous solvent; 5'. The method of producing aluminum iso propoxid'e- diresinate- which comprises reacting aluminum- trii‘sopropoxid'e- and rosin crystals in the proportion of‘ 1 mol of aluminum triiso propoxide-to 2 mols-of rosin crystals in- the pres ence- of‘ an- anhydrous» solvent, distilling off the alcohol setv free, and recovering‘ aluminum iso propoxide diresinate fromather solution. 6: The method of producing’ aluminum iso propoxider diresinate: which comprises; reacting aluminum triisopropoxide and‘hydrogenat'ed'rosin in the proportion‘ of 1 mol of aluminum trii'so propoxide to 2 mols‘off hydrogenated rosin in the 30 presence of an anhydrous‘ solvent‘, distilling‘ off the: alcohol‘ set‘ free, and‘ recovering- aluminum isopropoxide diresinate from theisolution. 12. The method of‘ producing‘ aluminum iso propoxide diresinate which. comprises. reacting 35 under anhydrous conditions aluminum triiso propoxide with rosin in the- proportion of‘ 1-‘ mol of' aluminum triisopropoxide to' 2 mols. of" resin, contacting the‘ aluminum isopropoxidel diresinate so- formed with‘ anhydrous isopropyl‘ alcohol and under anhydrous conditions aluminum, triiso propoxide. and; polymerized; rosin; in the: propor tion of L molv Ofi aluminum‘ triisopropoxide. to. 2 40 separatingtsaid aluminum isoprop'oxide'diresinate mols ofv polymerizedrosin. 7. The method of producing a1uminum_ iso propoxida diresinate,» which comprises, reacting in a puri?ed, state as a residue insoluble in said isopropyl alcohol. HAROLD M. SPURLIN.