CN101130676A - Adhesion promotion agent of composite metal caprate - Google Patents
Adhesion promotion agent of composite metal caprate Download PDFInfo
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- CN101130676A CN101130676A CNA2006100475580A CN200610047558A CN101130676A CN 101130676 A CN101130676 A CN 101130676A CN A2006100475580 A CNA2006100475580 A CN A2006100475580A CN 200610047558 A CN200610047558 A CN 200610047558A CN 101130676 A CN101130676 A CN 101130676A
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- zinc
- nickel
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- metal
- caprate
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Abstract
The invention discloses a composite metal caprate adhesive promotion agent for metal-rubber adhesion and method, which comprises the following steps: choosing cobalt sulfate, soda, solvent oil, new capric acid as raw material; adding one or several calcium or zinc nickel metallic compound into reactant; producing basic carbonate; washing the residue to without CO32-SO42-; reacting humid basic carbonate, new capric acid and so one organic acid in the solvent oil with reacting temperature between 40 deg. c and 230 deg. c; reacting for 16-24 h; reaching the reacting temperature to 90+-5 deg. c; adding into the metallic oxide; azeotropic-dewatering at 97-140 deg. c; dividing water; refluxing; reclaiming dissolvent at 140-180 deg. c; vacuum-evaporating relict dissolvent and water at 180+-5 deg. c; getting the product. This invention can decrease the preparing cost greatly.
Description
Technical field
The present invention relates to a kind of adhesion promotion agent of composite metal caprate and preparation method, this promotor is mainly used in the bonding of metal-rubber.
Background technology
Heat vulcanization type metal-rubber adhesion the promotor that uses on the domestic and international market is single metal-cobalt salt type product at present, along with cobalt metal price on the world market rises steadily, the cobalt salt adhesion promotion agent price also improves thereupon, therefore, reduce the cost of manufacture of cobalt salt adhesion promotion agent, become the research topic of numerous enterprises of going together, but do not see the relevant report that solves this difficult problem, can realize commercial operations so far yet.
Summary of the invention
The objective of the invention is with other metal part substituted metal cobalt, the preparation adhesion promotion agent of composite metal caprate, reducing the cost of manufacture of this adhesionpromoter, every technical indicator of product of the present invention all reaches or is higher than single cobalt salt type product; Another object of the present invention provides the preparation method of this adhesion promotion agent of composite metal caprate.
In order to realize above-mentioned purpose, the present invention is compatible with one or more metallic compounds and the inorganic cobalt salt of calcic, zinc, nickel, obtains containing cobalt 50～80%, contains the composite metal salt type adhesionpromoter of other metal 20～50%, promptly saves cobalt 20～50%.Reaction raw materials of the present invention comprises inorganic cobalt salt, soda ash, solvent oil, neodecanoic acid and C such as rose vitriol or cobalt chloride
2～C
18One or more mixtures of other organic acid is characterized in that adding at least the metallic compound of a kind of calcic and/or zinc and/or nickel in reactant, make adhesion promotion agent of composite metal caprate.
The further technical scheme of the present invention is: the metallic compound of calcium, zinc, nickel is calcium with the metal molar ratio of cobalt salt in promotor: zinc: nickel: cobalt=0～0.2: 0～0.05: 0～0.5: 0.5～0.8, calculate with pure metal, the weight ratio of each element is a calcium: zinc: nickel: cobalt=0～8: 0～3: 0～29: 29～48.The metallic compound of calcium, zinc, nickel is selected calcium oxide, zinc oxide and single nickel salt respectively for use.C
2～C
18Organic acid is selected one or more mixtures wherein such as acetate, propionic acid, sad, valeric acid, neodecanoic acid, naphthenic acid, stearic acid, sylvic acid, isocaprylic acid for use, and solvent oil is selected 80～200# gasoline for use.
The present invention makes adhesion promotion agent of composite metal caprate, and selected raw material and weight part proportioning are:
1, capric acid composite metal salt adhesion improver
Calcium oxide 0～10 zinc oxide 0～9 single nickel salt 0～100
Rose vitriol 170～225 calcined soda for industry 70～130 140# industrial napthas 300
Neodecanoic acid 105～360 valeric acids 10～90 acetate 5～40.
The preparation method of product of the present invention carries out as follows:
(1) rose vitriol or rose vitriol and single nickel salt is water-soluble, the processing industry soda ash aqueous solution is made the subcarbonate precipitation, and throw out is washed to no CO
3 2-SO
4 2-Standby;
(2) will wet subcarbonate directly and neodecanoic acid and other organic acid in solvent oil, react 40～230 ℃ of temperature of reaction, 16～24 hours reaction times;
(3) choosing adds metal oxide when temperature of reaction reaches 90 ± 5 ℃, in 97～140 ℃ of azeotropic dehydrations, divides water to reflux, and reclaims solvents in 140～180 ℃, and 180 ± 5 ℃ of vacuum steam residual solvent and moisture content obtains the composition metal caprate.
The present invention is that example and traditional capric acid cobalt compare with the composition metal caprate, and the every engineering test data of adherent are as follows between test brass-plated steel wire and the rubber:
| Test event | The capric acid cobalt | Invention composition metal caprate |
| Mooney viscosity M L(1+4)，100℃ | 78 | 76 |
| Mooney scorch, min T 3 T 18 | 11.02 15.04 | 9.28 14.20 |
| 151 ℃ of sulphur become instrument | ||
| M L，dNm | 2.83 | 3.02 |
| M 11，dNm | 25.13 | 26.72 |
| T 10，min | 2.56 | 2.54 |
| T 50，min | 6.21 | 6.06 |
| T 90，min | 14.40 | 14.32 |
| Vulcanizating glue physical performance (151 ℃) | 20 minutes 30 minutes 40 minutes | 20 minutes 30 minutes 40 minutes |
| Hardness, (Shao A) | 72 72 73 | 72 73 74 |
| Elongation, % | 411 398 397 | 421 385 391 |
| Tension set, % | 21 20 19 | 23 19 20 |
| Tensile strength at yield, MPa | 26.2 25.8 23.9 | 25.0 24.0 24.7 |
| 100% tensile modulus, MPa | 4.2 4.2 4.3 | 4.3 4.2 4.4 |
| 300% tensile modulus, MPa | 18.8 18.6 18.2 | 18.7 19.2 18.0 |
| Tear strength KN/m | 118 | 118 |
| Steel wire is extracted out, N | 1228 | 1210 |
| Flex crack, revolution * 10, mm | ||
| 300 | 7.9 | 8.0 |
| 750 | 14.2 | 14.1 |
| 1800 | 18.0 | 18.2 |
| 5000 | 19.1 | 19.0 |
| 100,000 fatigues | ||
| Elongation, % | 370 | 368 |
| Tensile strength at yield, MPa | 24.4 | 24.9 |
| 100 ℃ * 48h thermo-oxidative ageing | ||
| Elongation, % | 130 | 130 |
| Tensile strength at yield, MPa | 14.1 | 14.1 |
| Tear strength, KN/m | 39 | 38 |
| Steel wire is extracted out, N | 1201 | 1210 |
The invention provides following examples and describe its technical scheme in detail.
Embodiment 1: the proportioning of adhesion promotion agent of composite metal caprate (contain cobalt 80%＜weight in the composition metal 〉)
Embodiment 2:
(1) rose vitriol or rose vitriol and single nickel salt is water-soluble, the processing industry soda ash aqueous solution is made the subcarbonate precipitation, and throw out is washed to no CO
3 2-SO
4 2-Standby;
(2) will wet subcarbonate directly and capric acid and other organic acid in solvent oil, react 40～230 ℃ of temperature of reaction, 16～24 hours reaction times;
(3) choosing adds metal oxide when temperature of reaction reaches 90 ± 5 ℃, in 97～140 ℃ of azeotropic dehydrations, divides water to reflux water and solvent azeotropic in the time of 97 ℃.In order to make filter cake homodisperse in solvent oil, but the proper extension churning time is carried out total reflux operation; Begin branch water and reflux when filter cake is uniformly dispersed, be warming up to 140 ℃, moisture content separates fully substantially; Reclaim solvents in 140～180 ℃, 180 ± 5 ℃ of vacuum steam residual solvent and moisture content obtains the composition metal caprate.
Claims (5)
1. adhesion promotion agent of composite metal caprate, reaction raw materials comprises rose vitriol, soda ash, solvent oil, neodecanoic acid and C
2～C
18One or more mixtures of other organic acid is characterized in that adding at least the metallic compound of a kind of calcic and/or zinc and/or nickel in reactant.
2. according to the described composite metal salt adhesion improver of claim 1, the metallic compound that it is characterized in that calcium, zinc, nickel is calcium with the metal molar ratio of cobalt salt in promotor: zinc: nickel: cobalt=0～0.2: 0～0.05: 0～0.5: 0.5～0.8, calculate with pure metal, the weight ratio of each element is a calcium: zinc: nickel: cobalt=0～8: 0～3: 0～29: 29～48.
3. according to claim 1 or 2 described composite metal salt adhesion improvers, it is characterized in that the metallic compound of described calcium, zinc, nickel is selected calcium oxide, zinc oxide and single nickel salt respectively for use.
4. according to the described adhesion promotion agent of composite metal caprate of claim 1, it is characterized in that of the raw material reaction preparation of this promotor by following weight part:
Calcium oxide 0～10 zinc oxide 0～9 single nickel salt 0～100
Rose vitriol 170～225 calcined soda for industry 70～130 140# industrial napthas 300
Neodecanoic acid 105～360 valeric acids 10～90 acetate 5～40.
5. method for preparing adhesion promotion agent of composite metal caprate as claimed in claim 4 is characterized in that this method carries out as follows:
(1) rose vitriol or rose vitriol and single nickel salt is water-soluble, the processing industry soda ash aqueous solution is made the subcarbonate precipitation, and throw out is washed to no CO
3 2-SO
4 2-Standby;
(2) will wet subcarbonate directly and the organic acid of neodecanoic acid class in solvent oil, react 40～230 ℃ of temperature of reaction, 16～24 hours reaction times;
(3) choosing adds metal oxide when temperature of reaction reaches 90 ± 5 ℃, in 97～140 ℃ of azeotropic dehydrations, divides water to reflux, and reclaims solvents in 140～180 ℃, and 180 ± 5 ℃ of vacuum steam the caprate that residual solvent and moisture content obtain composition metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100475580A CN101130676A (en) | 2006-08-24 | 2006-08-24 | Adhesion promotion agent of composite metal caprate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100475580A CN101130676A (en) | 2006-08-24 | 2006-08-24 | Adhesion promotion agent of composite metal caprate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101130676A true CN101130676A (en) | 2008-02-27 |
Family
ID=39128083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100475580A Pending CN101130676A (en) | 2006-08-24 | 2006-08-24 | Adhesion promotion agent of composite metal caprate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101130676A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041851A (en) * | 2019-05-08 | 2019-07-23 | 大连爱柏斯化工股份有限公司 | The novel new cobalt decanoate adhesion promotor that a kind of viscosity is strong, cobalt content is low |
-
2006
- 2006-08-24 CN CNA2006100475580A patent/CN101130676A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041851A (en) * | 2019-05-08 | 2019-07-23 | 大连爱柏斯化工股份有限公司 | The novel new cobalt decanoate adhesion promotor that a kind of viscosity is strong, cobalt content is low |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20080227 |