US2294287A - Cobalt resinate and method of - Google Patents
Cobalt resinate and method of Download PDFInfo
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- US2294287A US2294287A US2294287DA US2294287A US 2294287 A US2294287 A US 2294287A US 2294287D A US2294287D A US 2294287DA US 2294287 A US2294287 A US 2294287A
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- United States
- Prior art keywords
- cobalt
- rosin
- hydrogenated rosin
- resinate
- hydrogenated
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title description 128
- 229910052803 cobalt Inorganic materials 0.000 title description 128
- 239000010941 cobalt Substances 0.000 title description 128
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 192
- 238000006243 chemical reaction Methods 0.000 description 32
- 150000001869 cobalt compounds Chemical class 0.000 description 30
- 239000002253 acid Substances 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 14
- VSGNNIFQASZAOI-UHFFFAOYSA-L Calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 12
- 239000001639 calcium acetate Substances 0.000 description 12
- 235000011092 calcium acetate Nutrition 0.000 description 12
- 229960005147 calcium acetate Drugs 0.000 description 12
- 230000003197 catalytic Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 239000011780 sodium chloride Substances 0.000 description 12
- QAHREYKOYSIQPH-UHFFFAOYSA-L Cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 10
- 229940011182 cobalt acetate Drugs 0.000 description 10
- 230000004927 fusion Effects 0.000 description 10
- 229920000591 gum Polymers 0.000 description 8
- 238000005984 hydrogenation reaction Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002023 wood Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- -1 alkali metal salt Chemical class 0.000 description 6
- 230000000903 blocking Effects 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- LBFUKZWYPLNNJC-UHFFFAOYSA-N Cobalt(II,III) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 159000000007 calcium salts Chemical class 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- PJQDFOMVKDFESH-UHFFFAOYSA-N cobalt(2+);N-(9H-fluoren-2-yl)-N-oxidoacetamide Chemical class [Co+2].C1=CC=C2C3=CC=C(N([O-])C(=O)C)C=C3CC2=C1.C1=CC=C2C3=CC=C(N([O-])C(=O)C)C=C3CC2=C1 PJQDFOMVKDFESH-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 238000002845 discoloration Methods 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000002736 metal compounds Chemical class 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000007500 overflow downdraw method Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000002966 varnish Substances 0.000 description 4
- 229960000583 Acetic Acid Drugs 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N Furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive Effects 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- XCGBFXNVKPHVEQ-UHFFFAOYSA-N cobalt;2,3-dihydroxybutanedioic acid;ethane-1,2-diamine Chemical compound [Co].NCCN.NCCN.NCCN.OC(=O)C(O)C(O)C(O)=O XCGBFXNVKPHVEQ-UHFFFAOYSA-N 0.000 description 2
- SKNKUZQQLUNPGJ-UHFFFAOYSA-N cobalt;formic acid Chemical compound [Co].OC=O SKNKUZQQLUNPGJ-UHFFFAOYSA-N 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000001419 dependent Effects 0.000 description 2
- 230000003292 diminished Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 229910000286 fullers earth Inorganic materials 0.000 description 2
- 238000007499 fusion processing Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 230000001264 neutralization Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 230000002269 spontaneous Effects 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
- C09F9/00—Compounds to be used as driers (siccatives)
Definitions
- This invention relates to the production of fused cobalt resinates and more particularly to fused cobalt resinates of improved characteristics and to the method of production thereof.
- Cobalt salts of wood or gum rosin have found wide usage as driers in paints and varnishes. Such salts have been made either by a precipitation method involving double decomposition of an alkali metal salt of rosin with a suitable'cobalt compound, or by a fusion process involving fusion of the rosin with a reactive cobalt compound.
- the precipitation method it has been possible to produce cobalt resinates containing up to the theoretical cobalt content for the neutral salt.
- the fusion method it has been impossible to introduce more than about 3% of cobalt due to the fact that blocking of the resinate occurs when about that amount of cobalt has become combined. For this reason the cobalt resinates produced commercially are usually prepared by the precipitation method. While such a method is more costly than the fusion method it has provided the only means of obtaining the desired higher cobalt contents.
- the above objects may be accomplished in accordance with this invention by fusing a hydrogenated rosin with a suiiicient amount of a cobalt compound capable of reaction with the hydrogenated rosin, at a temperature in the range of about 200 C. to about 350 C. to give a cobalt resinate of the hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin based on its acidity and as high as about 18% by weight.
- cobalt resinates containing more than the theoretical combining proportion of cobalt based on the acidity of the rosin .and up to about twice the theoretical cobalt content of cobalt diresinate are made available.
- a hydrogenated rosin is'reacted with a cobalt compound capable of reaction therewith to provide a salt.
- a cobalt compound capable of reaction therewith to provide a salt.
- a compound may, be-a basic cobalt compound or it may be a cobalt salt of a volatile we'ak acid or any other cobalt compound which under the fusion conditions liberates its cobalt.
- Suitable cobalt compounds are, for example, cobalt acetate, cobalt formate;----- 'rosin, ,of calcium acetate or other fatty acid salt of calcium or a fatty acid salt of zinc, lead, manganese, etc., may be employed, if desired in conjunction with the cobalt compound.
- the reaction is carried out by heating the hydrogenated rosin to a temperature in the range of about 200 C. to about 340 C. and adding the cobalt compound alone or in admixture with a catalytic meta1 compound such as a calcium salt either gradually or at one time, preferably while agitating the mixture.
- a catalytic meta1 compound such as a calcium salt
- the time of reaction required to combine the reactive cobalt compound with the hydrogenated I rosin to produce the high metal content fused cobalt resinates is dependent on the temperature employed, the particular cobalt compound used,
- reaction time may be varied from about minutes to several hours. It will be desirable to conduct the reaction in an inert atmosphere such as may be provided by carbon dioxide, nitrogen, etc., toprevent oxidation and discoloration of the hydrogenated rosin or the resinate at the elevated temperatures employed.
- the hydrogenated rosin which may be employed in the process of the invention may be produced, as is well known in the art, by contacting wood or gum rosin or the acids contained therein with hydrogen and a suitable hydrogenation catalyst.
- a hydrogenated product useful in this invention will beobtained.
- Hydrogenated rosin may also be obtained by contacting rosin dissolved in a suitable solvent with hydrogen and a noble metal hydrogenation catalyst, as for example platinum, palladium, etc., as is well known in the art.
- the hydrogenated rosin obtained by any of the above methods will have varying degrees'of saturation depending on the actual conditiohs'employed;
- a hydrogenated rosin having a saturation value corresponding to at least about 50 per cent saturation of both double 'bonds of the rosin acid contained in the rosin will be preferred, although rosins of lower saturation may also be employed.
- Hydrogenated rosins having a saturation of about 50 to about 95 per cent of both double bonds will be particularly desirable in the production of the novel resinates of the invention.
- the hydrogenated rosin may be subjected to vacuum distillation to remove the light end or to separate 'any particular fraction. If desired, it may be sub-.
- Example I one hundred parts by weight of a hydrogenated wood rosin saturated to the extent oi 63% 01- both double bonds of the rosin acid contained there- ,in and having an acid number of 158 and a drop melting point of 75 C. were melted and heated to a temperature of 240 C. in a nitrogen atmosphere.
- a mixture of 86 parts by weight of cobalt Example II One hundred and ten parts by weight of hydrogenated gum rosin having a saturation of 60% of both double bonds of the rosin acid contained therein, an acid number oi 155 anda drop melt- -ing point of 79 C. were melted and heated to'a above about 100 and preferably from about 135 to about 185.
- fused cobalt salts of hydrogenated rosin described in accordance with this invention will be considerably more useful in the commercial fields such as for example, as driers in paints or varnishes, in plastics, adhesives, printing inks,
- Example III in Example I 400 parts by weight of the rosin were melted and heated to a temperature of 280 C. in a carbon dioxide atmosphere. A mix ture of 167 parts by weight of cobalt acetate and 36 parts by weight of calcium acetate was then added gradually in small portions at a time with agitation. The reaction temperature was raised gradually to a maximum of 310 C. during the addition. A total addition time of 70 minutes was employed. The cobalt resinate obtained had a drop melting point of 200 C., a cobalt content of 9%, and a calcium content of 2%.
- a cobalt resinate of' a hydrogenated wood rosin having a cobalt content greater than the equivalent combining proportion of the hydro-.
- the method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight which comprises fusing a hydrogenated rosin with a cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufficient to give a resinate of the above defined cobalt content at a temperagigge within the range of about 200 C. to about 6.
- the method of producing a cobalt resinate of a, hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight which comprises fusing a hydrogenated rosin'with a. cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufficient to give a resinate of the above defined cobalt content and in the presence of a catalytic metal compound at a temperature within the range of about 200 C. to about 350 C.
- the method of producing a cobalt resinate of a, hydrogenated rosin having a cobalt content greater than the equivalent combining porportion of the hydrogenated rosin but not in excess of about 18% by weight which comprises fusing a hydrogenated rosin with a cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufiicient to give a resinate of the above defined cobalt content and in the presence of a small amount of a calcium salt as catalyst at a. temperature within the range of about 200 C. to about 350 C.
- the method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight which comprises fusing'a hydrogenated .rosin with cobalt acetate in an amount suflicient to give a resinate of the above defined cobalt content and in the presence of a small amount of calcium acetate'as catalyst at a temperature within the range of about 275 C. to about 330 C.
- the method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight which comprises fusing a hydrogenated rosin with a mixture of cobalt oxide and aceticacid in an amount sufiicient to give a resinate of the above defined cobalt content and in the presence of a small amount of calcium acetate as catalyst at a temperature within the range of about 275 C. to about 330 C.
Description
Patented Aug. 25, 1942 COBALT masma'ra AND METHOD OF PRODUCING Herschel Elliottrwilmington, DeL, lssignol' to Hercules Powder Company, Wilmington, Del., a corporationof Delaware No Drawing. Application September 4, 1941,
Serial llo. 409,537
11 Claims. (01. 260100) This invention relates to the production of fused cobalt resinates and more particularly to fused cobalt resinates of improved characteristics and to the method of production thereof.
Cobalt salts of wood or gum rosin have found wide usage as driers in paints and varnishes. Such salts have been made either by a precipitation method involving double decomposition of an alkali metal salt of rosin with a suitable'cobalt compound, or by a fusion process involving fusion of the rosin with a reactive cobalt compound. By the precipitation method it has been possible to produce cobalt resinates containing up to the theoretical cobalt content for the neutral salt. By the fusion method, however, it has been impossible to introduce more than about 3% of cobalt due to the fact that blocking of the resinate occurs when about that amount of cobalt has become combined. For this reason the cobalt resinates produced commercially are usually prepared by the precipitation method. While such a method is more costly than the fusion method it has provided the only means of obtaining the desired higher cobalt contents.
It is an object of this invention to provide fused cobalt resinates of higher cobalt content than has been heretofore possible.
It is another object to provide fused cobalt resinates of high cobalt content which possess many improved characteristics.
g It is a further object to provide a method of producing fused cobalt resinates of higher cobalt content than has been heretofore possible.
Other objects of the invention will appear hereinafter.
The above objects may be accomplished in accordance with this invention by fusing a hydrogenated rosin with a suiiicient amount of a cobalt compound capable of reaction with the hydrogenated rosin, at a temperature in the range of about 200 C. to about 350 C. to give a cobalt resinate of the hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin based on its acidity and as high as about 18% by weight. The theoretical cobalt content of a hydrogenated rosin in place of ordinary rosin and according to the, described procedure, that clear homogeneous resinates may be prepared without the blocking disadvantage encountered in the production of cobalt resinates from ordinary rosins. Thus, by the process of this invention cobalt resinates containing more than the theoretical combining proportion of cobalt based on the acidity of the rosin .and up to about twice the theoretical cobalt content of cobalt diresinate are made available.
In carrying out the fusion process-oftfi in vention a hydrogenated rosin is'reacted with a cobalt compound capable of reaction therewith to provide a salt. Such a compound may, be-a basic cobalt compound or it may be a cobalt salt of a volatile we'ak acid or any other cobalt compound which under the fusion conditions liberates its cobalt. Suitable cobalt compounds are, for example, cobalt acetate, cobalt formate;----- 'rosin, ,of calcium acetate or other fatty acid salt of calcium or a fatty acid salt of zinc, lead, manganese, etc., may be employed, if desired in conjunction with the cobalt compound.
The reaction is carried out by heating the hydrogenated rosin to a temperature in the range of about 200 C. to about 340 C. and adding the cobalt compound alone or in admixture with a catalytic meta1 compound such as a calcium salt either gradually or at one time, preferably while agitating the mixture. When the catalytic metal compound is used, satisfactory fusion takes 1 place at temperatures as low as 200 C. but when the catalytic material is not employed it is usually desirable to employ a fusion temperature of at least about 275 C. At lower temperatures without the, catalytic material there is a slight tendency to blocking in passing through the reaction stage representing formation of a resinate containing about 3 to 10% of combined cobalt. Considerable foaming accompanies the reaction and it is therefore preferable to agitate during the addition and to carry out the addition 7 W over an extended period. The foaming is-more severe at the lower temperatures and reaction As a catalytic V ends from the hydrogenated rosin. tures of about 275 to about 330 C. are therefore becomes diminished due to volatilization of light Temperapreferable' for the reaction.
The time of reaction required to combine the reactive cobalt compound with the hydrogenated I rosin to produce the high metal content fused cobalt resinates is dependent on the temperature employed, the particular cobalt compound used,
\ 'the degree of agitation, the particular amount of metal being introduced, as well as on other factors. Thus, the reaction time may be varied from about minutes to several hours. It will be desirable to conduct the reaction in an inert atmosphere such as may be provided by carbon dioxide, nitrogen, etc., toprevent oxidation and discoloration of the hydrogenated rosin or the resinate at the elevated temperatures employed.
The hydrogenated rosin which may be employed in the process of the invention may be produced, as is well known in the art, by contacting wood or gum rosin or the acids contained therein with hydrogen and a suitable hydrogenation catalyst. Thus, by contacting rosin in a fluid condition with hydrogen in the presence of an activated base metal hydrogenation catalyst under a pressure in the range of about 200 to 15,000 pounds per square inch and at a temperature of about 125 C. to about 225 C. a hydrogenated product useful in this invention will beobtained.
Hydrogenated rosin may also be obtained by contacting rosin dissolved in a suitable solvent with hydrogen and a noble metal hydrogenation catalyst, as for example platinum, palladium, etc., as is well known in the art. The hydrogenated rosin obtained by any of the above methods will have varying degrees'of saturation depending on the actual conditiohs'employed; For use in the present invention a hydrogenated rosin having a saturation value corresponding to at least about 50 per cent saturation of both double 'bonds of the rosin acid contained in the rosin will be preferred, although rosins of lower saturation may also be employed. Hydrogenated rosins having a saturation of about 50 to about 95 per cent of both double bonds will be particularly desirable in the production of the novel resinates of the invention. After hydrogenation the hydrogenated rosin may be subjected to vacuum distillation to remove the light end or to separate 'any particular fraction. If desired, it may be sub-.
jected to a refining treatmentwith a selective color-body solvent or absorbent as furfural, phenol, fullers earth, etc. The hydrogenated rosin used will generally havean acid number The following specific examples are illustrative oi the various embodiments oi the invention:
\ Example I one hundred parts by weight of a hydrogenated wood rosin saturated to the extent oi 63% 01- both double bonds of the rosin acid contained there- ,in and having an acid number of 158 and a drop melting point of 75 C. were melted and heated to a temperature of 240 C. in a nitrogen atmosphere. A mixture of 86 parts by weight of cobalt Example II One hundred and ten parts by weight of hydrogenated gum rosin having a saturation of 60% of both double bonds of the rosin acid contained therein, an acid number oi 155 anda drop melt- -ing point of 79 C. were melted and heated to'a above about 100 and preferably from about 135 to about 185.
The fused cobalt salts of hydrogenated rosin described in accordance with this invention will be considerably more useful in the commercial fields such as for example, as driers in paints or varnishes, in plastics, adhesives, printing inks,
etc., due to the improved characteristics over prior cobalt resinates. Thus, they will contain a higher cobalt content than has been possible heretofore, which is a very desired advantage. They will also be less subject to oxidation and discoloration at both normal and elevated temperatures and will also be less subject to spontaneous ignition than j the cobalt resinates prepared from ordinary rosin. They will be clear homogeneous resins and will be substantially free of precipitated or suspended matter.
temperature of 255 C. in a nitrogen atmosphere. A mixture 01' 71 parts by weight of cobalt acetate and 10 parts by weight of calcium acetate was then added gradually in small portions at a time with constant agitation and while permitting the reaction to subside before each subsequent addition. The reaction temperature was raised gradually during the addition to a maximum of 325 C. The fused cobalt resinate obtained had smelting point of 215 C., a cobalt content of 13.3% and a calicum content of 2%. It was a clear homogeneous resin.
Example III in Example I, 400 parts by weight of the rosin were melted and heated to a temperature of 280 C. in a carbon dioxide atmosphere. A mix ture of 167 parts by weight of cobalt acetate and 36 parts by weight of calcium acetate was then added gradually in small portions at a time with agitation. The reaction temperature was raised gradually to a maximum of 310 C. during the addition. A total addition time of 70 minutes was employed. The cobalt resinate obtained had a drop melting point of 200 C., a cobalt content of 9%, and a calcium content of 2%.
It will be understood that the details and examples hereinbefore set forth are illustrative only and that the invention as broadly described and claimed is in no way ted thereby.
What I claim and desire to protect by Letter Patent is:
1. A cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equiv alent combining proportion of the hydrogenated rosin'but not in excess of about 18% by weight. 2. A cobalt resinate of a hydrogenated rosin saturated to the extent of at least 50% of both double bonds of the rosin acid contained therein and having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight.
3'. A cobalt resinate of' a hydrogenated wood rosin having a cobalt content greater than the equivalent combining proportion of the hydro-.
2,294,287 genated rosin but not in excess of about 18%- by weight.
4. A cobalt resinate of a hydrogenated gum rosin having a, cobalt content greater than the equivalent combining proportion. of the hydrogenated rosin but not in excess of about 18% by weight.
5. The method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing a hydrogenated rosin with a cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufficient to give a resinate of the above defined cobalt content at a temperagigge within the range of about 200 C. to about 6. The method of producing a cobalt resinate of a, hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing a hydrogenated rosin'with a. cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufficient to give a resinate of the above defined cobalt content and in the presence of a catalytic metal compound at a temperature within the range of about 200 C. to about 350 C.
7. The method of producing a cobalt resinate of a, hydrogenated rosin having a cobalt content greater than the equivalent combining porportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing a hydrogenated rosin with a cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufiicient to give a resinate of the above defined cobalt content and in the presence of a small amount of a calcium salt as catalyst at a. temperature within the range of about 200 C. to about 350 C.
8. The method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing a hydrogenated rosin with a cobalt compound capable of reaction with the hydrogenated rosin, in an amount sufficient to give a resinate of the above defined cobalt content at a'temperature within the range of about 275 C. to about 330 C. d 9. The method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing'a hydrogenated .rosin with cobalt acetate in an amount suflicient to give a resinate of the above defined cobalt content and in the presence of a small amount of calcium acetate'as catalyst at a temperature within the range of about 275 C. to about 330 C.
10. The method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but notin excess of about 18% by weight, which comprises fusing a, hydrogenated rosin with a mixture of cobalt oxide and cobaltacetate in an amount suflicient to give a resinate of the above defined cobalt content and in the presence of a small amount of calcium acetate as catalyst at a temperature within the range of about 275 C. to about 330 C. a
11. The method of producing a cobalt resinate of a hydrogenated rosin having a cobalt content greater than the equivalent combining proportion of the hydrogenated rosin but not in excess of about 18% by weight, which comprises fusing a hydrogenated rosin with a mixture of cobalt oxide and aceticacid in an amount sufiicient to give a resinate of the above defined cobalt content and in the presence of a small amount of calcium acetate as catalyst at a temperature within the range of about 275 C. to about 330 C.
HERSCHEL A. ELLIOTT.
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| US2294287A true US2294287A (en) | 1942-08-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4340515A (en) * | 1981-06-16 | 1982-07-20 | Akzo Nv | Solid rubber adhesion promoter and a method for improving the adhesion of rubber to metal reinforcing elements embedded therein |
| WO2023099784A1 (en) | 2021-12-03 | 2023-06-08 | Umicore Specialty Materials Brugge | Liquid cobalt resinate compositions and methods of preparing the same |
-
0
- US US2294287D patent/US2294287A/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4340515A (en) * | 1981-06-16 | 1982-07-20 | Akzo Nv | Solid rubber adhesion promoter and a method for improving the adhesion of rubber to metal reinforcing elements embedded therein |
| WO2023099784A1 (en) | 2021-12-03 | 2023-06-08 | Umicore Specialty Materials Brugge | Liquid cobalt resinate compositions and methods of preparing the same |
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