CN103897216A - High-performance organic cobalt mixed salt and preparation method thereof - Google Patents
High-performance organic cobalt mixed salt and preparation method thereof Download PDFInfo
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- CN103897216A CN103897216A CN201410122639.7A CN201410122639A CN103897216A CN 103897216 A CN103897216 A CN 103897216A CN 201410122639 A CN201410122639 A CN 201410122639A CN 103897216 A CN103897216 A CN 103897216A
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Abstract
The invention discloses a high-performance organic cobalt mixed salt. The organic cobalt mixed salt is in a form of a bluish violet solid in light of the appearance, contains 15 to 16% of cobalt, and has the melting point of 103 to 104 DEG C. The organic cobalt mixed salt is prepared from the following raw materials in parts by weight: 26 to 28 parts of cobaltous hydroxide, 63 to 66 parts of stearic acid, 19 to 21 parts of propionic acid, 39 to 41 parts of isononanoic acid, 20 to 22 parts of boric butyl ester, and 8 to 9 parts of calcium metaborate. The high-performance organic cobalt mixed salt has the beneficial effects that propionic acid can greatly reduce the total acidity of the high-performance organic cobalt mixed salt, and thus a rubber product can be prevented from corroding and ageing; stearic acid added can effectively replace part of stearic acid that is commonly used in a tire formula, which is beneficial for the full dispersing of the main components of rubber (tire) like carbon black and zinc oxide; in addition, calcium metaborate added to cobalt salt is an amphoteric compound which can keep power of hydrogen balance in the system, and thus the corrosion resistance and cementing performance are improved, the adhering between rubber and metal is improved, and as a result, the cobalt content and reaction activity of such cobalt salt are greatly increased and improved.
Description
Technical field
The present invention relates to a kind of high-performance organic cobalt class mixing salt and preparation method thereof.
Background technology
Along with developing rapidly of China's motorway, the swift and violent increase of auto output, to increase considerably the demand of radial, the demand of the indispensable raw material-organic cobalt salt adhesion promotion agent to production radial is increasing so, more and more higher to specification of quality.For now, no matter be that domestic also external produced organic cobalt salt adhesion promotion agent is all the products that adopt cobalt to obtain from different organic acid reactions, belong to organic acid cobalt mixture, the content of cobalt is different by the product standard of the different trades mark, but in the time of the formulating of recipe of rubber item, the usage quantity of different organic cobalt salt adhesion promotion agents is to calculate with cobalt contents, the pure cobalt amount of namely occupying in every hundred umber rubber.Because organic cobalt adhesionpromoter action principle in application process is: organic cobalt salt adhesion promotion agent adds and is distributed to equably in whole system in mixing process, now just physical property is disperseed, in the time that rubber vulcanizes, there is replacement(metathesis)reaction with the coating surface of metallic surface at a certain temperature in organic cobalt salt adhesion promotion agent, generate the cobalt ion of free radical, between cobalt ion catalysis rubber and metal and sulphur, form stable chemical bond, reach the strong binding between rubber and metal, not only guarantee that tire has the performance of running at high speed, but also the work-ing life of prolongation tire.And cobalt is a kind of non-ferrous metal in organic cobalt salt adhesion promotion agent, it is again the little kind in non-ferrous metal, the not enough kiloton of cobalt that the whole nation produces from raw ore, most of dependence from external import cobalt ore, so the price of cobalt is all the time in high-end price, from cobalt salt adhesion promotion agent product, its cost accounts for 80% of total raw material price.Along with market competition is growing more intense under situation; cobalt salt adhesion promotion agent will become how much levels to increase on consumption; but price can proportionally not rise; although in existing cobalt salt adhesion promotion agent preparation method, cobalt boracylate is higher containing cobalt amount simultaneously; they are in the time of the vulcanization of rubber; reactive behavior is large; bonding enhancing to rubber and steel wire plays a major role; but the free fatty acids total acidity that reaction produces is higher; unfavorable rubber and steel wire bonding lasting; and metallic surface is corrosive, therefore research and development are extremely necessary for cobalt new raw material or novel process.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provide a kind of containing cobalt amount higher, to the favourable high-performance organic cobalt class mixing salt of anticorrosion tackify preparation method.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of high-performance organic cobalt class mixing salt, this organic cobalt class mixing salt outward appearance is bluish voilet solid, it is 15%～16% containing cobalt amount, fusing point is 103～104 ℃, and this organic cobalt class mixing salt forms by weight ratio by following raw material: 26～28 parts of cobaltous hydroxides, 63～66 parts of stearic acid, 19～21 parts of propionic acid, 39～41 parts of different n-nonanoic acids, 20～22 parts, boric acid fourth fat, 8～9 parts of calcium metaborates.
High-performance organic cobalt class mixing salt a preparation method, complete according to the following steps:
1) salt-forming reaction: take cobaltous hydroxide, propionic acid, different n-nonanoic acid and stearic mixing acid as raw material, in atmospheric pressure sealed container, 170～180 ℃ of temperature, reaction times >=2.5 hour, reaction generates propionic acid-cobalt stearate mixing salt, and its total reaction formula is:
Wherein, m is 8 or 17;
2) boron acylation reaction: in above-mentioned reaction system, add boric acid fourth fat, control 190～195 ℃ of temperature, reaction times >=2 hour, reaction generates cobalt boracylate, and byproduct is propionic acid fourth fat, and its reaction formula is:
Wherein, m is 8 or 17;
3) make finished product: in above-mentioned reaction system, temperature is controlled at 180～185 ℃, add calcium metaborate, make take cobalt boracylate as main organic cobalt class mixing salt finished product.
The temperature of described salt-forming reaction is 175 ℃.
The temperature of described boron acylation reaction is 193 ℃.
The described temperature of making finished product is 183 ℃.
A kind of high-performance cobalt class mixing salt, its each raw material preferred proportion is: 27 parts of cobaltous hydroxides, 65 parts of stearic acid, 20 parts of propionic acid, 40 parts of different n-nonanoic acids, 21 parts, boric acid fourth fat, 8.5 parts of calcium metaborates.
The invention has the beneficial effects as follows:
Propionic acid in the present invention greatly reduces product total acidity, and aging resistance corrosion-resistant to glue based article are avoided, simultaneously, the stearic acid adding in the present invention can effectively substitute part of stearic acid conventional in tire formulation, be conducive to carbon black, the abundant diffusion of the rubber such as zinc oxide (tire) main component, in addition, in cobalt salt, add calcium metaborate, calcium metaborate is a kind of two property compounds, potential of hydrogen in can active balance system, preservative property are improved, strengthen gumminess, promote the bonding of rubber and metal, thereby greatly improve this class cobalt salt containing cobalt amount and reactive behavior.
Embodiment
The present invention is further illustrated in conjunction with the embodiments now.
Embodiment mono-
A kind of high-performance organic cobalt class mixing salt, this organic cobalt class mixing salt outward appearance is bluish voilet solid, it is 15.2% containing cobalt amount, fusing point is 103 ℃, and this organic cobalt class mixing salt forms by weight ratio by following raw material: 26 parts of cobaltous hydroxides, 65 parts of stearic acid, 19 parts of propionic acid, 39 parts of different n-nonanoic acids, 20 parts, boric acid fourth fat, 8 parts of calcium metaborates.
High-performance organic cobalt class mixing salt a preparation method, complete according to the following steps:
1) salt-forming reaction: take cobaltous hydroxide, propionic acid, different n-nonanoic acid and stearic mixing acid as raw material, in atmospheric pressure sealed container, 175 ℃ of temperature, reaction times >=2.5 hour, reaction generates propionic acid-cobalt stearate mixing salt, and its total reaction formula is:
Wherein, m is 8 or 17;
2) boron acylation reaction: in above-mentioned reaction system, add boric acid fourth fat, control 193 ℃ of temperature, reaction times >=2 hour, reaction generates cobalt boracylate, and byproduct is propionic acid fourth fat, and its reaction formula is:
Wherein, m is 8 or 17;
3) make finished product: in above-mentioned reaction system, temperature is controlled at 183 ℃, add calcium metaborate, make take cobalt boracylate as main organic cobalt class mixing salt finished product.
Embodiment bis-
A kind of high-performance organic cobalt class mixing salt, this organic cobalt class mixing salt outward appearance is bluish voilet solid, it is 15.4% containing cobalt amount, fusing point is 103.5 ℃, and this organic cobalt class mixing salt forms by weight ratio by following raw material: 27 parts of cobaltous hydroxides, 65 parts of stearic acid, 20 parts of propionic acid, 40 parts of different n-nonanoic acids, 21 parts, boric acid fourth fat, 8.5 parts of calcium metaborates.
High-performance organic cobalt class mixing salt a preparation method, complete according to the following steps:
1) salt-forming reaction: take cobaltous hydroxide, propionic acid, different n-nonanoic acid and stearic mixing acid as raw material, in atmospheric pressure sealed container, 175 ℃ of temperature, reaction times >=2.5 hour, reaction generates propionic acid-cobalt stearate mixing salt, and its total reaction formula is:
Wherein, m is 8 or 17;
2) boron acylation reaction: in above-mentioned reaction system, add boric acid fourth fat, control 193 ℃ of temperature, reaction times >=2 hour, reaction generates cobalt boracylate, and byproduct is propionic acid fourth fat, and its reaction formula is:
Wherein, m is 8 or 17;
3) make finished product: in above-mentioned reaction system, temperature is controlled at 183 ℃, add calcium metaborate, make take cobalt boracylate as main organic cobalt class mixing salt finished product.
Embodiment tri-
A kind of high-performance organic cobalt class mixing salt, this organic cobalt class mixing salt outward appearance is bluish voilet solid, it is 15.6% containing cobalt amount, fusing point is 104 ℃, and this organic cobalt class mixing salt forms by weight ratio by following raw material: 28 parts of cobaltous hydroxides, 66 parts of stearic acid, 21 parts of propionic acid, 41 parts of different n-nonanoic acids, 22 parts, boric acid fourth fat, 9 parts of calcium metaborates.
High-performance organic cobalt class mixing salt a preparation method, complete according to the following steps:
1) salt-forming reaction: take cobaltous hydroxide, propionic acid, different n-nonanoic acid and stearic mixing acid as raw material, in atmospheric pressure sealed container, 175 ℃ of temperature, reaction times >=2.5 hour, reaction generates propionic acid-cobalt stearate mixing salt, and its total reaction formula is:
Wherein, m is 8 or 17;
2) boron acylation reaction: in above-mentioned reaction system, add boric acid fourth fat, control 193 ℃ of temperature, reaction times >=2 hour, reaction generates cobalt boracylate, and byproduct is propionic acid fourth fat, and its reaction formula is:
Wherein, m is 8 or 17;
3) make finished product: in above-mentioned reaction system, temperature is controlled at 183 ℃, add calcium metaborate, make take cobalt boracylate as main organic cobalt class mixing salt finished product.
Above-mentioned cobaltous hydroxide: molecular formula Co (OH)
2, molecular weight 93.
Proterties: Co (OH)
2pinkiness powder, water content < 2%,, at high temperature also can there is this variation in the meeting brown hydrous oxide of oxidized generation at leisure in air.
Above-mentioned propionic acid: molecular formula CH
3cH
2cOOH, molecular weight 74.
Proterties: colourless liquid, irritant smell, content >=99.5%, acid number 758mgKOH/g, proportion (d204 ℃) 0.9942, fusing point-20.8 ℃, 140.7 ℃ of boiling points, specific refractory power 1.3862, flash-point 1300F, can be miscible with water, is dissolved in ethanol, chloroform and ether.This product low toxicity.Stimulate eyes same with Glacial acetic acid, mucocutaneous, and have bactericidal properties, Dermallly affixed upper after, used water is rinsed, and has dressed face guard when operation, equipment will seal.
Above-mentioned stearic acid: molecular formula CH
3(CH
2)
16cOOH, molecular-weight average approximately 284.
Proterties: outward appearance is powder or the crystallinity lump that white or off-white color have soapy feeling, and its section has micro-fine needle crystal with gloss; There is the micro-smelly, tasteless of similar grease.This product is easily molten in chloroform or ether, in ethanol, dissolves, and almost insoluble in water, density is about 0.9408g/mL.
Above-mentioned different n-nonanoic acid: molecular formula is 3,5,5 tri-methyl hexanoic acids, molecular weight 158.2.
Proterties: outward appearance is the transparent liquid with any peculiar peculiar smell, zero pour: below-30 ℃, boiling point: 225 ℃, flash-point: 127 ℃, burning-point: 440 ℃, specific refractory power: 1.427.
Above-mentioned boric acid fourth fat: molecular formula C
12h
27bO
3, molecular weight 203.16,
Proterties: outward appearance is colourless transparent liquid, and density is about 0.8530g/mL, refractive index 1.407,230 ℃ of boiling points, easily moist, can be miscible with the common solvent such as methyl alcohol, meet water decomposition.
Above-mentioned calcium metaborate: molecular formula Ca (BO
2)
26H
2o, molecular weight 233.7.
Proterties: white inorganic salt, Powdered, 160 ℃ lose above crystal water, are both sexes.
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, relevant staff can, not departing from the scope of this invention technological thought, carry out various change and modification completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to claim scope.
Claims (6)
1. a high-performance organic cobalt class mixing salt, it is characterized in that, this organic cobalt class mixing salt outward appearance is bluish voilet solid, it is 15%～16% containing cobalt amount, fusing point is 103～104 ℃, and this organic cobalt class mixing salt forms by weight ratio by following raw material: 26～28 parts of cobaltous hydroxides, 63～66 parts of stearic acid, 19～21 parts of propionic acid, 29～31 parts of different n-nonanoic acids, 20～22 parts, boric acid fourth fat, 8～9 parts of calcium metaborates.
A kind of high-performance organic cobalt class mixing salt according to claim 1 preparation method, it is characterized in that, complete according to the following steps:
1) salt-forming reaction: take cobaltous hydroxide, propionic acid, different n-nonanoic acid and stearic mixing acid as raw material, in atmospheric pressure sealed container, 170～180 ℃ of temperature, reaction times >=2.5 hour, reaction generates propionic acid-cobalt stearate mixing salt, and its total reaction formula is:
Wherein, m is 8 or 17;
2) boron acylation reaction: in above-mentioned reaction system, add boric acid fourth fat, control 190～195 ℃ of temperature, reaction times >=2 hour, reaction generates cobalt boracylate, and byproduct is propionic acid fourth fat, and its reaction formula is:
Wherein, m is 8 or 17;
3) make finished product: in above-mentioned reaction system, temperature is controlled at 180～185 ℃, add calcium metaborate, make take cobalt boracylate as main organic cobalt class mixing salt finished product.
A kind of high-performance organic cobalt class mixing salt according to claim 2 preparation method, it is characterized in that, the temperature of described salt-forming reaction is 175 ℃.
A kind of high-performance organic cobalt class mixing salt according to claim 2 preparation method, it is characterized in that, the temperature of described boron acylation reaction is 193 ℃.
A kind of high-performance organic cobalt class mixing salt according to claim 2 preparation method, it is characterized in that, the described temperature of making finished product is 183 ℃.
6. a kind of high-performance organic cobalt class mixing salt according to claim 1, is characterized in that, its each raw material preferred proportion is: 27 parts of cobaltous hydroxides, 65 parts of stearic acid, 20 parts of propionic acid, 30 parts of different n-nonanoic acids, 21 parts, boric acid fourth fat, 8.5 parts of calcium metaborates.
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|---|---|---|---|
| CN201410122639.7A CN103897216A (en) | 2014-03-28 | 2014-03-28 | High-performance organic cobalt mixed salt and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011369A (en) * | 2017-04-18 | 2017-08-04 | 江阴市三良橡塑新材料有限公司 | A kind of preparation method of high-performance compound cobalt boracylate |
| CN109942895A (en) * | 2019-03-26 | 2019-06-28 | 江阴市三良橡塑新材料有限公司 | A kind of organic cobalt salt and preparation method thereof having white carbon black divergent function |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0148782A1 (en) * | 1984-01-10 | 1985-07-17 | Manchem Limited | Adhesion promoter improving the adhesion of rubber to metals |
| CN1844213A (en) * | 2006-04-10 | 2006-10-11 | 徐美华 | Process for preparing organic cobalts mixed salt finished product with cobalt neodecanoate as main raw material |
| CN101003544A (en) * | 2007-01-16 | 2007-07-25 | 徐美华 | Method for preparing finished products of salt mixture of organic cobalt class of giving priority to cobalt boroacidate |
-
2014
- 2014-03-28 CN CN201410122639.7A patent/CN103897216A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0148782A1 (en) * | 1984-01-10 | 1985-07-17 | Manchem Limited | Adhesion promoter improving the adhesion of rubber to metals |
| CN1844213A (en) * | 2006-04-10 | 2006-10-11 | 徐美华 | Process for preparing organic cobalts mixed salt finished product with cobalt neodecanoate as main raw material |
| CN101003544A (en) * | 2007-01-16 | 2007-07-25 | 徐美华 | Method for preparing finished products of salt mixture of organic cobalt class of giving priority to cobalt boroacidate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011369A (en) * | 2017-04-18 | 2017-08-04 | 江阴市三良橡塑新材料有限公司 | A kind of preparation method of high-performance compound cobalt boracylate |
| CN109942895A (en) * | 2019-03-26 | 2019-06-28 | 江阴市三良橡塑新材料有限公司 | A kind of organic cobalt salt and preparation method thereof having white carbon black divergent function |
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Application publication date: 20140702 |