CN101864088B - Preparation method of compound type cobalt stearate adhesion promoter - Google Patents
Preparation method of compound type cobalt stearate adhesion promoter Download PDFInfo
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- CN101864088B CN101864088B CN201010201667XA CN201010201667A CN101864088B CN 101864088 B CN101864088 B CN 101864088B CN 201010201667X A CN201010201667X A CN 201010201667XA CN 201010201667 A CN201010201667 A CN 201010201667A CN 101864088 B CN101864088 B CN 101864088B
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Abstract
The invention discloses a preparation method of a compound type cobalt stearate adhesion promoter, comprising the following steps of: converting inorganic dissoluble cobalt salt into precipitant cobalt which is not easy to dissolve in water; reacting precipitant cobalt powder with composite organic weak acid in an organic solvent for 10-18 hours; raising the reaction temperature to stearic acid melting temperature from room temperature with the speed of 20-30 DEG C/h; raising the reaction temperature to 140 DEG C at the speed of 20 DEG C/h; then, remaining 2 hours at the temperature of 140 DEG C, wherein the composite organic acid is a mixture of stearic acid, isocaprylic acid and abietic acid;, steaming the residual organic solvent after the reaction is finished; and pelleting to obtain the compound type cobalt stearate adhesion promoter. In the compound type cobalt stearate adhesion promoter prepared by the preparation method, the cobalt content can completely satisfy standard requirements, and the reaction conditions are reduced, thereby the energy consumption is reduced. Meanwhile, because the organic acid with low molecular weight and branched chains is used, the service performance of the compound type cobalt stearate adhesion promoter is increased, and the binding performance and the ageing resistance of the compound type stearate adhesion promoter are particularly outstanding.
Description
Technical field
The invention belongs to field of material engineering technology, be specifically related to the preparation method of compound type cobalt stearate adhesion promoter.
Background technology
Strengthen rubber item industries such as travelling belt, Rubber Hose Braided With Steel Wire at radial wire cord tire, steel wire, need elastomerics such as rubber and metallic framework material high-tenacity bonding.Prior art adopts direct addition type organic cobalt salt adhesion promotion agent (mainly comprising cobalt stearate, cobalt naphthenate, capric acid cobalt and cobalt boracylate four big classes) usually; And cobalt stearate is by single Triple Pressed Stearic Acid and inorganic cobalt direct reaction gained; Its product has following shortcoming in application process: 1, the Triple Pressed Stearic Acid of technical grade is the mixture of straight chain octadecane alkyl sfas and n-Hexadecane alkyl sfas; The Triple Pressed Stearic Acid octadecane alkyl saturated fatty acid content of one-level is between 64-78%; So its molecular-weight average is 276; Have only 9.7% with this highest theoretical content of calculating cobalt stearate, the cobalt contents in the cobalt stearate that on market, circulates at present is basically all between 9.0-9.6%, and is bigger with the higher limit gap of standard-required.And cobalt contents is low and organic acid is bigger, and this plays the adhesion promotion effect to it in sizing material unfavorable, and because of mainly playing the cobalt ion that has only of bonding enhancement effect, organic acid is equivalent to impurity composition and is left in the rubber item in rubbery system.2, because Triple Pressed Stearic Acid is the straight chain hydrocarbon saturated acid, so its chain rupture energy than the height of branched-chain hydrocarbon, so in reaction system, be difficult for separating with cobalt ion, discharges the cobalt ion of radical.3, since used stearic acidity a little less than, for make reaction more fully in reaction process controlled temperature higher, energy consumption is bigger.In view of above some, develop a kind of compound cobalt stearate, both satisfied index request, improve use properties again, also cut down the consumption of energy simultaneously.
Summary of the invention
Technical problem to be solved by this invention is through the improvement to the cobalt stearate compound method, thereby solves the unmanageable problem of its technical indicator and improve its use properties.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of preparation method of compound type cobalt stearate adhesion promoter, this method comprises the steps:
(1) inorganic solubility cobalt salt is dissolved in water; The configuration cobalt concentration reaches the cobalt liquor (to contain pure cobalt amount) of 15～45g/L; Configuration concentration is that sodium hydroxide solution and the concentration of 100～300g/L is the sodium carbonate solution of 150～300g/L respectively again, and above-mentioned three kinds of solution are subsequent use after filtering respectively;
(2) cobalt liquor is heated to 85 ± 5 ℃, under the agitation condition, slowly adds temperature and be 40～50 ℃ sodium hydroxide solution; When the pH of reaction solution value is 7, under the agitation condition, slowly add temperature again and be 40～50 ℃ sodium carbonate solution; When the pH of reaction solution value is 9.5; Stop to add sodium carbonate solution, holding temperature continues to be stirred to the pH value and does not change at 50～60 ℃;
(3) reaction solution that step (2) is obtained leaves standstill, and gets deposition and uses water rinse, reaches 7 until the pH of rinsing liquid value;
(4) rinsing is the good inorganic cobalt salt of deposition carries out the dehydration first time, and its water cut is reached below 50%;
(5) will adopt the rotary flashing drying system to carry out the dehydration second time through the inorganic cobalt salt of deposition after the dehydration for the first time;
The inorganic cobalt salt of deposition that (6) will pass through twice dehydration reacted 10～18 hours with the compound organic monoacid in organic solvent; Described compound organic monoacid is Triple Pressed Stearic Acid, isocaprylic acid and sylvic acid, and mol ratio is 1.5～1.7: 0.24～0.30: 0.11～0.20; Be specially: after adding sylvic acid and immiscible organic solvent earlier in the reaction kettle; The inorganic cobalt salt of deposition that will pass through twice dehydration adds and mixes, and drops into Triple Pressed Stearic Acid when the speed of 20～30 ℃/h is warmed up to the Triple Pressed Stearic Acid melting temperature, continues to be warmed up to 80～110 ℃ with the speed of 20 ℃/h; Slowly drop into isocaprylic acid afterwards; Making time was controlled at 0.5～2 hour, kept 2 hours after being warming up to 140 ℃ with the speed of 20 ℃/h then, was about 10～18 hours from being dosed into the discharging entire reaction time;
(7) after the reaction of step (6) finishes, steam remaining organic solvent, carry out granulation, obtain the compound type cobalt stearate adhesion promoter product.
Inorganic solubility cobalt salt described in the step (1) is rose vitriol, NSC 51149 or Xiao Suangu.
Agitation condition when adding sodium hydroxide solution in the step (2) is 50～60rpm; Agitation condition when adding sodium carbonate solution is 20～40rpm.
Centrifugal or filter pressing mode is adopted in the described dehydration first time of step (4).
In the step (5), the time of adopting the rotary flashing drying system to carry out dehydration for the second time is no more than 5 seconds, promptly is prone to oxidized divalent cobalt ion in the moment dehydration; Hightail oxidized environment, avoid the divalence cobalt to be oxidized to the trivalent cobalt, in dehumidification system, cut simultaneously with air-flow; So the cobalt powder particle is a primary particle; Not only particle is little, and loose, and tap density has only 0.4～0.5g/cm
3, water content is less than 3%, and the trivalent cobalt contents is less than 0.1%; Has higher chemical reactivity; Examine under a microscope this type of cobalt powder, find that each small-particle surface all has numerous aperture, cobalt powder that this present invention just produces and the conventional cobalt powder difference of making.
Organic solvent described in the step (6) is a YLENE.
The inorganic cobalt salt of deposition and compound organic faintly acid mol ratio are 1: 2.00～2.05 in the step (6).
Patent of the present invention is the improvement to existing patent " preparation method of organic cobalt salt adhesion promotion agent " (application number 200910025533.4, on 02 09th, 2009 applying date).The method of manufacture of cobalt stearate is to use single Triple Pressed Stearic Acid in existing patent; Cobalt contents in its product is the highest can only to reach 9.6%; And require in the standard between 9.0-10.2%, be impossible though in the standard-required scope, will reach higher limit, because of present commercially available one-level Triple Pressed Stearic Acid average weight between 274-278; If with the main acid of this acid as the production cobalt stearate; So products obtained therefrom in theory cobalt contents between 9.61-9.74%, but, guarantee to react and carry out to such an extent that will have a kind of material excessive fully because this kind reaction is weak acid and weakly alkaline reaction; And cobalt is rare valuable metallic element; So will excessive acid in order to guarantee that cobalt all converts organic cobalt to, cobalt contents does not just reach ideal value in the product under the situation of excessive acid, so the cobalt contents of the cobalt stearate that circulates on the market now is all between 9.0-9.6%.And compound type cobalt stearate adhesion promoter of the present invention is to have adopted three kinds of acid strong and weak organic acids that do not wait to carry out suitable composite and inorganic cobalt to react; Be better than the acid organic acid existence of Triple Pressed Stearic Acid so under the lower situation of cobalt concentration, also be prone to combine because have with cobalt; Institute is so that speed of response and efficient raising; Reduce temperature of reaction, this just need not use high boiling organic solvent.
Beneficial effect: the compound type cobalt stearate adhesion promoter that produces through the inventive method; Wherein cobalt contents not only satisfies standard-required fully; Thereby and reduced reaction conditions and reduced energy consumption; So simultaneously since its use properties of organic acid of having used small molecular weight and having had a side chain also increase, especially particularly outstanding aspect bond properties and ageing resistance.
Can know that from the patent of application number 200910025533.4 the bonding of rubber and metal mainly is to make the copper of metallic surface and the sulphur in the rubbery system form Cu by the divalent cobalt ion with katalysis that organic cobalt salt provides
xS, Cu
xS again with rubber in the combining of sulphur, form stable chemical bond (Cu
x-S-S
y-Rub), have very strong bounding force between rubber and the intermetallic thereby make.So, more its promoter actions of the divalent cobalt ion that in the raw material with aliquot, provides are just strong more, and the cobalt contents in the product of the present invention can reach higher limit, and just cobalt contents is higher than cobalt contents in the cobalt stearate product.Its two because divalent cobalt ion is to combine with organic acid in product, not only need patent as application number 200910025533.4 in said effective cobalt many; Promptly there is not the trivalent cobalt; And plant therewith a little less than divalence cobalt bonded chemical bond also needs, could more be prone to discharge free divalence cobalt, and what in the manufacturing processed of before cobalt stearate, adopt is the octadecyl acid of straight chain hydrocarbon; Because of it is that straight chain hydrocarbon is so bond energy is higher; Discharge the exigent energy of radical cobalt ion, and compound stearate acid cobalt greatly reduces organic acid and cobalt bonded energy owing to adopted the organic acid that has side chain of Compositional type; Thereby more be prone to discharge more cobalt ion, strengthen the adhesion promotion ability.Its three owing to used the acid organic acid that does not wait, make the reaction conditions reduction, in the time of 140 ℃, just can react completely, so with an organic solvent do not need high boiling solvent.Its four because the difference of organic acid is also different to the corrosive nature of metallic framework material; Organic acid in the compound cobalt stearate partly is a branched acids, and its molecular weight is little, and is stronger with the affinity of rubber; Reduce it to the Corrosion of Metallic Materials effect, thereby prolong the ageing resistance of rubber.
Embodiment
According to following embodiment, can understand the present invention better.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used to explain the present invention, and the present invention that should also can not limit in claims to be described in detail.
Embodiment 1:
(1) inorganic solubility cobalt salt is dissolved in water; The configuration cobalt concentration reaches the cobalt liquor (to contain pure cobalt amount) of 15～45g/L; Configuration concentration is that sodium hydroxide solution and the concentration of 100～300g/L is the sodium carbonate solution of 150～300g/L respectively again, and above-mentioned three kinds of solution are subsequent use after filtering respectively;
(2) cobalt liquor is heated to 85 ± 5 ℃, under the agitation condition, slowly adds temperature and be 40～50 ℃ sodium hydroxide solution; When the pH of reaction solution value is 7, under the agitation condition, slowly add temperature again and be 40～50 ℃ sodium carbonate solution; When the pH of reaction solution value is 9.5; Stop to add sodium carbonate solution, holding temperature continues to be stirred to the pH value and does not change at 50～60 ℃;
(3) reaction solution that step (2) is obtained leaves standstill, and gets deposition and uses water rinse, reaches 7 until the pH of rinsing liquid value;
(4) rinsing is the good inorganic cobalt salt of deposition carries out the dehydration first time, and its water cut is reached below 50%;
(5) will adopt the rotary flashing drying system to carry out second time and dewater through the inorganic cobalt salt of deposition after the dehydration for the first time, process water cut less than 5% cobalt powder;
(6) add earlier in the reaction kettle sylvic acid and the xylene solvent of 62.7kg miscible after; The 151.5kg cobalt powder that step (5) is made adds mixing; When being warmed up to Triple Pressed Stearic Acid melting temperature (about 70 ℃), the speed of 30 ℃/h drops into the 567kg Triple Pressed Stearic Acid, and slower because of the more weak speed of response of stearic acidity, be raised to 80～110 ℃ so will expect the temperature continuation with the speed of 20 ℃/h; At this moment speed of response is accelerated greatly; 2～3 hours basic total overall reactions are arranged generally speaking, slowly drop into the 49kg isocaprylic acid afterwards in confined conditions, making time was controlled between 0.5～2 hour; For guaranteeing the material total overall reaction, will expect to keep 2 hours after temperature is brought up to 140 ℃ with the speed of 20 ℃/h.Be about 16 hours from being dosed into the discharging entire reaction time;
(7) after the reaction of step (6) finishes, steam remaining organic solvent, can adopt vacuum distillation, carry out granulation after solvent is all steamed system, obtain the compound type cobalt stearate adhesion promoter product for accelerating purifying velocity.Its physicochemical property parameter is seen table 1.
The physicochemical property parameter of the compound type cobalt stearate adhesion promoter product that table 1 embodiment 1 makes
| Project | Standard index | Analysis indexes |
| Outward appearance | Hyacinthine or red-purple are granular | Red-purple is granular |
| The cobalt mass percent, % | 9.6±0.6 | 10.1 |
| Softening temperature, ℃ | 80～100 | 94 |
| Ash content mass percent (550 ℃), %<= | 13.4 | 13.2 |
| Weight loss on heating (105 ℃, 2h), %<= | 2.0 | 0.20 |
| Density, g/cm 3 | 1.09±0.03 | 1.12 |
| Ir spectra (reference standard collection of illustrative plates) | Comparable | Comparable |
Embodiment 2:
Method with embodiment 1; The difference that adds material quantity in the step (6) that different is: the sylvic acid that adds 48.8kg in the reaction kettle earlier mixes with the 151.5kg cobalt powder adding that step (5) is made after xylene solvent is miscible; When being warmed up to Triple Pressed Stearic Acid melting temperature (about 70 ℃), the speed of 30 ℃/h drops into the 603.5kg Triple Pressed Stearic Acid; Slowly drop into the 29kg isocaprylic acid afterwards in confined conditions; Making time was controlled between 0.5～2 hour, for guaranteeing the material total overall reaction, will expect that temperature brings up to 140 ℃ with the speed of 20 ℃/h and kept 2 hours.
Its physicochemical property parameter is seen table 2.
The physicochemical property parameter of the compound type cobalt stearate adhesion promoter product that table 2 embodiment 2 makes
| Project | Standard index | Analysis indexes |
| Outward appearance | Hyacinthine or red-purple are granular | Red-purple is granular |
| The cobalt mass percent, % | 9.6±0.6 | 9.4 |
| Softening temperature, ℃ | 80～100 | 89 |
| Ash content mass percent (550 ℃), %<= | 13.4 | 13.0 |
| Weight loss on heating (105 ℃, 2h), %<= | 2.0 | 0.20 |
| Density, g/cm 3 | 1.09±0.03 | 1.00 |
| Ir spectra (reference standard collection of illustrative plates) | Comparable | Comparable |
Embodiment 3 (Comparative Examples):
Step (1)-(5) and step (7) are identical with embodiment 1, and different is step (6).
Be specially: the 151.5kg cobalt powder that will make reacts with the 720kg Triple Pressed Stearic Acid in industrial naptha (boiling point is at 150-175 ℃) environment; When temperature of reaction below 100 ℃ the time; Heat up with the speed of 30 ℃/h,, heat up with the speed of 5 ℃/h when temperature of reaction during at 100～140 ℃; When temperature of reaction during at 140～160 ℃, the control TRT, reaction finished when temperature reaches 160 ℃, approximately is 20 hours from being dosed into the discharging reaction times at 4 hours.
The organic cobalt salt adhesion promotion agent product (cobalt stearate) that makes, its physicochemical property parameter is seen table 3.
The physicochemical property parameter of the cobalt stearate that table 3 embodiment 3 makes
| Project | Standard index | Analysis indexes |
| Outward appearance | Hyacinthine or red-purple are granular | Red-purple is granular |
| The cobalt mass percent, % | 9.6±0.6 | 9.4 |
| Softening temperature, ℃ | 80～100 | 91 |
| Ash content mass percent (550 ℃), %<= | 13.4 | 13.01 |
| Weight loss on heating (105 ℃, 2h), %<= | 2.0 | 0.45 |
| Density, g/cm 3 | 1.09±0.03 | 1.10 |
| Ir spectra (reference standard collection of illustrative plates) | Comparable | Comparable |
Embodiment 4: the application test of product.
Embodiment 1～3 resulting three products are made sizing material respectively, and all raw material consumptions are all consistent in formula system, survey glue bond.Testing method is (a H extraction method).The result sees table 4.
Table 4
Claims (5)
1. the preparation method of a compound type cobalt stearate adhesion promoter is characterized in that this method comprises the steps:
(1) inorganic solubility cobalt salt is dissolved in water; To contain the cobalt liquor that pure cobalt amount configuration cobalt concentration reaches 15～45g/L; Configuration concentration is that sodium hydroxide solution and the concentration of 100～300g/L is the sodium carbonate solution of 150～300g/L respectively again, and above-mentioned three kinds of solution are subsequent use after filtering respectively;
(2) cobalt liquor is heated to 85 ± 5 ℃, under the agitation condition, slowly adds temperature and be 40～50 ℃ sodium hydroxide solution; When the pH of reaction solution value is 7, under the agitation condition, slowly add temperature again and be 40～50 ℃ sodium carbonate solution; When the pH of reaction solution value is 9.5; Stop to add sodium carbonate solution, holding temperature continues to be stirred to the pH value and does not change at 50～60 ℃;
(3) reaction solution that step (2) is obtained leaves standstill, and gets deposition and uses water rinse, reaches 7 until the pH of rinsing liquid value;
(4) rinsing is the good inorganic cobalt salt of deposition carries out the dehydration first time, and its water cut is reached below 50%;
(5) will adopt the rotary flashing drying system to carry out the dehydration second time through the inorganic cobalt salt of deposition after the dehydration for the first time;
The inorganic cobalt salt of deposition that (6) will pass through twice dehydration reacted 10～18 hours with the compound organic monoacid in organic solvent; Described compound organic monoacid is Triple Pressed Stearic Acid, isocaprylic acid and sylvic acid, and mol ratio is 1.5～1.7: 0.24～0.30: 0.11～0.20; Be specially: after adding sylvic acid and immiscible organic solvent earlier in the reaction kettle; The inorganic cobalt salt of deposition that will pass through twice dehydration adds and mixes, and drops into Triple Pressed Stearic Acid when the speed of 20～30 ℃/h is warmed up to the Triple Pressed Stearic Acid melting temperature, continues to be warmed up to 80～110 ℃ with the speed of 20 ℃/h; Slowly drop into isocaprylic acid afterwards; Making time was controlled at 0.5～2 hour, kept 2 hours after being warming up to 140 ℃ with the speed of 20 ℃/h then, and be 10～18 hours from being dosed into the discharging entire reaction time;
(7) after the reaction of step (6) finishes, steam remaining organic solvent, carry out granulation, obtain the compound type cobalt stearate adhesion promoter product;
Agitation condition when adding sodium hydroxide solution in the step (2) is 50～60rpm; Agitation condition when adding sodium carbonate solution is 20～40rpm;
The inorganic cobalt salt of deposition and compound organic faintly acid mol ratio are 1: 2.00～2.05 in the step (6).
2. the preparation method of compound type cobalt stearate adhesion promoter according to claim 1 is characterized in that the inorganic solubility cobalt salt described in the step (1) is rose vitriol, NSC 51149 or Xiao Suangu.
3. the preparation method of compound type cobalt stearate adhesion promoter according to claim 1 is characterized in that the centrifugal or filter pressing mode of step (4) the described first time of dehydration employing.
4. the preparation method of compound type cobalt stearate adhesion promoter according to claim 1 is characterized in that the time of adopting the rotary flashing drying system to carry out dehydration for the second time in the step (5) is no more than 5 seconds.
5. the preparation method of compound type cobalt stearate adhesion promoter according to claim 1 is characterized in that the organic solvent described in the step (6) is a YLENE.
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| CN102807485B (en) * | 2011-06-01 | 2015-05-13 | 深圳市格林美高新技术股份有限公司 | Composite cobalt salt bonding promoter and preparation method thereof |
| CN102336925B (en) * | 2011-07-07 | 2012-10-10 | 江阴市三良化工有限公司 | Method for preparing compound fatty acid cobalt salt |
| CN102702573B (en) * | 2012-06-01 | 2013-09-04 | 江苏卡欧化工有限公司 | Preparation method of environment-friendly compound adhesion promoter |
| CN103113206A (en) * | 2012-12-31 | 2013-05-22 | 大连爱柏斯化工有限公司 | Preparation method of neodecanoic acid cobalt |
| CN104788718B (en) * | 2015-04-15 | 2017-07-18 | 江阴市三良橡塑新材料有限公司 | A kind of high stability new cobalt decanoate mixing salt production process |
| CN110759825A (en) * | 2019-11-11 | 2020-02-07 | 山东阳谷华泰化工股份有限公司 | Synthesis method of cobalt stearate |
| CN114456441A (en) * | 2022-01-26 | 2022-05-10 | 江苏卡欧化工股份有限公司 | Cobalt stearate adhesive and preparation method thereof |
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