CN110055009A - The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low - Google Patents
The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low Download PDFInfo
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- CN110055009A CN110055009A CN201910378984.XA CN201910378984A CN110055009A CN 110055009 A CN110055009 A CN 110055009A CN 201910378984 A CN201910378984 A CN 201910378984A CN 110055009 A CN110055009 A CN 110055009A
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- adhesion promotor
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- cobaltous
- cobaltous octadecanate
- chloride
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- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 28
- 239000010941 cobalt Substances 0.000 title claims abstract description 28
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 30
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims abstract description 30
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical class Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 28
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 10
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 10
- -1 cobaltous chlorides Chemical class 0.000 claims abstract description 9
- 230000000694 effects Effects 0.000 claims abstract description 8
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 4
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000012986 modification Methods 0.000 claims abstract description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 28
- 239000007864 aqueous solution Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000012153 distilled water Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 12
- 229940097267 cobaltous chloride Drugs 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical class [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 8
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229910000162 sodium phosphate Inorganic materials 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000000605 extraction Methods 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 244000061458 Solanum melongena Species 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention relates to cobaltous octadecanate adhesion promotor preparation technical fields, and disclose the novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low, raw material including following parts by weight proportion: 150 parts of odium stearate, 20.5~24 parts of waterless cobaltous chlorides, 8~11.5 parts of Dehydrated nickel chlorides, 3~4 parts of sodium tripolyphosphates, 5~10 parts of thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；Preparation method are as follows: by under the dispersion adjustment effect of sodium tripolyphosphate, replace the divalent cobalt ion of a part using bivalent nickel ion, realize the modification to cobaltous octadecanate, again with after cure stabilizer thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is sufficiently compound, and novel cobaltous octadecanate adhesion promotor is prepared.The present invention solves cobaltous octadecanate adhesion promotor in the prior art, while reducing cobaltous octadecanate production cost by reducing the cobalt content in cobaltous octadecanate to reach, cannot achieve the technical issues of effectively improving its adhesion promotion performance in rubbery system.
Description
Technical field
The present invention relates to cobaltous octadecanate adhesion promotor preparation technical field, specially a kind of viscosity is strong, cobalt content is low
Novel cobaltous octadecanate adhesion promotor.
Background technique
Cobaltous octadecanate is the indispensable raw material for producing radial wire cord tire, main work as a kind of adhesion promotor
With mechanism are as follows: during refining glue, cobaltous octadecanate is added in rubber system, and makes the cobaltous octadecanate be in rubber system
Physical homogeneously dispersed state, when raw rubber is vulcanized, cobaltous octadecanate is set with metal surface coating at a certain temperature
Reaction is changed, free radical divalent cobalt ion is generated, the free radical divalent cobalt ion released makes rubber elastomer by catalytic action
Stable chemical bond is formed between metallic framework material and sulphur to realize mutual high-tenacity adhesive effect.
Wherein, the cobalt content in cobaltous octadecanate is only between 9.0%~10.0%, however cobalt is small as a kind of Yield comparison
And expensive small kind non-ferrous metal, the Costco Wholesale of itself account for the 80% of cobaltous octadecanate total price cost, and therefore, control
Cobalt content in cobaltous octadecanate processed can play the purpose of effectively control cobaltous octadecanate total price cost；Although stearic by reducing
Cobalt content in sour cobalt can play the purpose for reducing cost of material, but cobalt content is low in cobaltous octadecanate, stearate radical content
High composed structure, plays that adhesion promotion is unfavorable to it in sizing material because mainly serve adhesion promotion only have cobalt from
Son, stearate radical only just correspond to impurity component in rubbery system.How in cobaltous octadecanate is effectively reduced cobalt content it is same
When, realization effectively improves its adhesion promotion performance in rubbery system, becomes the key technical problem for needing to solve at present.
The present invention provides the novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low, it is intended to solve existing skill
Cobaltous octadecanate adhesion promotor in art is being produced by reducing the cobalt content in cobaltous octadecanate with reaching reduction cobaltous octadecanate
This while, cannot achieve the technical issues of effectively improving its adhesion promotion performance in rubbery system.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the novel cobaltous octadecanate adhesion promotion that the present invention provides a kind of viscosity by force, cobalt content is low
Agent solves cobaltous octadecanate adhesion promotor in the prior art, is reaching drop by reducing the cobalt content in cobaltous octadecanate
While low cobaltous octadecanate production cost, it cannot achieve and effectively improve the technology of its adhesion promotion performance in rubbery system and ask
Topic.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low, the raw material including following parts by weight proportion:
150 parts of odium stearate, 20.5~24 parts of waterless cobaltous chlorides, 8~11.5 parts of Dehydrated nickel chlorides, 3~4 parts of sodium tripolyphosphates, 5~10
Part thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of above-mentioned adhesion promotor makes the following steps are included: by under the dispersion adjustment effect of sodium tripolyphosphate
Replace the divalent cobalt ion of a part with bivalent nickel ion, realize modification to cobaltous octadecanate, then with after cure stabilizer
Thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is sufficiently compound, and novel cobaltous octadecanate adhesion promotor is prepared；
Or the raw material including following parts by weight proportion: 20 parts of stearic acid, 1865,2.2 parts of cobalt hydroxides, 1 part of nickel hydroxide, 6
Part thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；Above-mentioned stearic acid, at vacuum degree -0.08MPa, in cobalt hydroxide
Divalent cobalt ion and nickel hydroxide in bivalent nickel ion acid-base neutralization reaction directly occurs, generate novel cobaltous octadecanate, then
It is sufficiently compound with after cure stabilizer thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt, it is viscous that novel cobaltous octadecanate is prepared
Close promotor.
Preferably, the adhesion promotor includes the raw material of following parts by weight proportion: 150g odium stearate, 20.5g without
Water cobalt chloride, 11.5g Dehydrated nickel chloride, 3g sodium tripolyphosphate, 10g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
Preferably, the adhesion promotor includes the raw material of following parts by weight proportion: 150g odium stearate, 23.5g without
Water cobalt chloride, 8.5g Dehydrated nickel chloride, 3.5g sodium tripolyphosphate, 5g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
Preferably, the adhesion promotor includes the raw material of following parts by weight proportion: 150g odium stearate, 24g are anhydrous
Cobalt chloride, 8g Dehydrated nickel chloride, 4g sodium tripolyphosphate, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
Preferably, the adhesion promotor preparation method the following steps are included:
S1. 150 parts of odium stearate are dissolved in the distilled water that 1L temperature is 60~90 DEG C, it is water-soluble that preparation obtains odium stearate
Liquid, which is placed at 60~90 DEG C keep the temperature it is spare；
S2. 20.5~24 parts of waterless cobaltous chlorides are dissolved in 200~300mL distilled water, preparation obtains cobalt chloride solution；
S3. 8~11.5 parts of Dehydrated nickel chlorides are dissolved in 100mL distilled water, preparation obtains nickel chloride aqueous solution；
S4. the nickel chloride aqueous solution in the cobalt chloride solution and step S3 in step S2 is added and is counted equipped with agitating device, PH
In the reactor of heating device, 3~4 parts of sodium tripolyphosphates are added into reactor will be in step S1 under heating stirring
Aqueous solution of sodium stearate is added drop-wise in reactor, and during the reaction by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise
So that the pH value of solution in reactor is remained alkalinity, after being added dropwise, be added 5~10 parts of thiosulfuric acids S, S'-1,6- oneself two
Alcohol ester disodium salt stops heating and stirring operation, the mixed system in reactor is filtered later, removes filtrate, preparation
Obtain flocky precipitate；
S5. the sediment in step S4 is washed using distilled water, until it can't detect chloride ion；
S6. the sediment in step S5 is placed in vacuum oven, is taken out after dry 6~8h at 105~120 DEG C, it is cooling
To room temperature, the sieve of 100 mesh numbers is crossed after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
Preferably, in the step S4, made instead by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise during the reaction
The pH value of solution in device is answered to remain at 9~10.
Preferably, in the step S4, made instead by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise during the reaction
The pH value of solution in device is answered to remain at 9.5.
Preferably, in the step S4, at stirring rate 300r/min, 70 DEG C of heating temperature, with the dropwise addition speed of 5mL/s
Aqueous solution of sodium stearate is added in reactor by rate.
Preferably, it in the step S4, puts the precipitate in vacuum oven, the dry 7h at 110 DEG C.
Preferably, the adhesion promotor includes the raw material of following parts by weight proportion: 150g odium stearate, 24g are anhydrous
Cobalt chloride, 8g Dehydrated nickel chloride, 4g sodium tripolyphosphate, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention by under the dispersion adjustment effect of sodium tripolyphosphate, using bivalent nickel ion replace the divalent cobalt of a part from
Son is realized the modification to cobaltous octadecanate, then is filled with after cure stabilizer thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt
It is point compound, novel cobaltous octadecanate adhesion promotor is prepared；Wherein, nickel and cobalt belong to " chalophile element " in geochemistry,
It is similarly in the VIIIth B race of the 4th period, they have similar electron structure, and [schematic atomic diagram of cobalt is (+27) 2,8,15,2；
The schematic atomic diagram of nickel is (+28) 2,8,16,2], bivalent nickel ion replaces the divalent cobalt ion of a part in theory, together
Sample can complete the adhesion promotion mechanism of action of divalent cobalt ion, and nickel cost of material is well below cobalt raw material, is cobalt class raw material valence
The 1/4~1/3 of lattice；
Alternatively, stearic acid, at vacuum degree -0.08MPa, with the divalent in the divalent cobalt ion and nickel hydroxide in cobalt hydroxide
Acid-base neutralization reaction directly occurs for nickel ion, generates novel cobaltous octadecanate, then with after cure stabilizer thiosulfuric acid S, S'-1,6-
Hexylene glycol ester disodium salt is sufficiently compound, and novel cobaltous octadecanate adhesion promotor is prepared；
It is 6.49~6.83% by the cobalt content in the novel cobaltous octadecanate adhesion promotor prepared of the test present invention, and it is right
The cobalt content of the novel cobaltous octadecanate prepared in ratio is compared for 9.4%, and achieving significantly reduces in cobaltous octadecanate adhesion promotor
The technical effect of cobalt content；
The novel cobaltous octadecanate adhesion promotor prepared in the present invention and comparative example is fabricated to full steel wire heavy load radial wheel
The belt sizing material of tire, autohesion of the present invention is 33~34N, extraction force is 861~878N, extraction force after 100 DEG C × 48h aging
It is taken compared with extraction force 673N after the autohesion 25N of comparative example, extraction force 764N, 100 DEG C × 48h aging for 789~811N
Obtained the technical effect for significantly improving the adhesion promotion performance of cobaltous octadecanate adhesion promotor.
Specific embodiment
Embodiment one:
Novel cobaltous octadecanate adhesion promotor includes following raw material: 150g odium stearate, 20.5g waterless cobaltous chloride, 11.5g are anhydrous
Nickel chloride, 3g sodium tripolyphosphate, 10g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of novel cobaltous octadecanate adhesion promotor the following steps are included:
S101. 150g odium stearate is dissolved in the distilled water that 1L temperature is 60 DEG C, preparation obtains aqueous solution of sodium stearate, will
The aqueous solution of sodium stearate be placed at 60 DEG C keep the temperature it is spare；
S102. 20.5g waterless cobaltous chloride is dissolved in 200mL distilled water, preparation obtains cobalt chloride solution；
S103. 11.5g Dehydrated nickel chloride is dissolved in 100mL distilled water, preparation obtains nickel chloride aqueous solution；
S104. the nickel chloride aqueous solution in the cobalt chloride solution and step S103 in step S102 is added equipped with stirring dress
Set, PH meter and heating device reactor in, into reactor be added 3g sodium tripolyphosphate, stirring rate 300r/min, plus
Under hot temperature 60 C, the aqueous solution of sodium stearate in step S101 is added in reactor with the drop rate of 5mL/s, and
The pH value of solution in reactor is set to remain at 9 by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise in reaction process, drop
After adding, 10g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is added, later, stops heating and stirring operation, it will be anti-
It answers the mixed system in device to be filtered, removes filtrate, flocky precipitate is prepared；
S105. the sediment in step S104 is washed using distilled water, until it can't detect chloride ion；
S106. the sediment in step S105 is placed in vacuum oven, is taken out after dry 8h at 105 DEG C, is cooled to room
Temperature crosses the sieve of 100 mesh numbers after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
Embodiment two:
Novel cobaltous octadecanate adhesion promotor includes following raw material: 150g odium stearate, 23.5g waterless cobaltous chloride, 8.5g are anhydrous
Nickel chloride, 3.5g sodium tripolyphosphate, 5g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of novel cobaltous octadecanate adhesion promotor the following steps are included:
S201. 150g odium stearate is dissolved in 1L distilled water at a temperature of 90 °C, preparation obtains aqueous solution of sodium stearate, will
The aqueous solution of sodium stearate be placed at 90 DEG C keep the temperature it is spare；
S202. 23.5g waterless cobaltous chloride is dissolved in 250mL distilled water, preparation obtains cobalt chloride solution；
S203. 8.5g Dehydrated nickel chloride is dissolved in 100mL distilled water, preparation obtains nickel chloride aqueous solution；
S204. the nickel chloride aqueous solution in the cobalt chloride solution and step S203 in step S202 is added equipped with stirring dress
Set, PH meter and heating device reactor in, into reactor be added 3.5g sodium tripolyphosphate, stirring rate 300r/min,
At 80 DEG C of heating temperature, the aqueous solution of sodium stearate in step S201 is added in reactor with the drop rate of 5mL/s, and
Remain at the pH value of solution in reactor by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise during the reaction
10, after being added dropwise, 5g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is added, later, stops heating and stirring operation,
Mixed system in reactor is filtered, filtrate is removed, flocky precipitate is prepared；
S205. the sediment in step S204 is washed using distilled water, until it can't detect chloride ion；
S206. the sediment in step S205 is placed in vacuum oven, is taken out after dry 6h at 120 DEG C, is cooled to room
Temperature crosses the sieve of 100 mesh numbers after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
Embodiment three:
Novel cobaltous octadecanate adhesion promotor includes following raw material: 150g odium stearate, 24g waterless cobaltous chloride, the anhydrous chlorination of 8g
Nickel, 4g sodium tripolyphosphate, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of novel cobaltous octadecanate adhesion promotor the following steps are included:
S301. 150g odium stearate is dissolved in the distilled water that 1L temperature is 80 DEG C, preparation obtains aqueous solution of sodium stearate, will
The aqueous solution of sodium stearate be placed at 80 DEG C keep the temperature it is spare；
S302. 24g waterless cobaltous chloride is dissolved in 300mL distilled water, preparation obtains cobalt chloride solution；
S303. 8g Dehydrated nickel chloride is dissolved in 100mL distilled water, preparation obtains nickel chloride aqueous solution；
S304. the nickel chloride aqueous solution in the cobalt chloride solution and step S303 in step S302 is added equipped with stirring dress
Set, PH meter and heating device reactor in, into reactor be added 4g sodium tripolyphosphate, stirring rate 300r/min, plus
Under hot temperature 70 C, the aqueous solution of sodium stearate in step S301 is added in reactor with the drop rate of 5mL/s, and
The pH value of solution in reactor is set to remain at 9.5 by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise in reaction process,
After being added dropwise, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is added, later, stops heating and stirring operation, it will be anti-
It answers the mixed system in device to be filtered, removes filtrate, flocky precipitate is prepared；
S305. the sediment in step S304 is washed using distilled water, until it can't detect chloride ion；
S306. the sediment in step S305 is placed in vacuum oven, is taken out after dry 7h at 110 DEG C, is cooled to room
Temperature crosses the sieve of 100 mesh numbers after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
Example IV:
Novel cobaltous octadecanate adhesion promotor includes following raw material: 20kg stearic acid 1865,2.2kg cobalt hydroxide, 1kg hydroxide
Nickel, 6g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of novel cobaltous octadecanate adhesion promotor the following steps are included:
S401. 20kg stearic acid 1865,10kg dimethylbenzene are added in reaction kettle, start high-speed stirring apparatus, is in revolving speed
Under 200rpm, slowly 2.2kg cobalt hydroxide and 1kg nickel hydroxide are added in reaction kettle；
S402. after adding cobalt hydroxide and nickel hydroxide, heating device is opened, when temperature rises to 95 DEG C, distillation discharge diformazan
Benzene and water；
S403. reaction kettle is warming up to 180 DEG C, and keeps the temperature 1h at 170 DEG C, later, be evaporated under reduced pressure, it is true in decompression process
Reciprocal of duty cycle is down to -0.08MPa from -0.01MPa, and 2h is kept at vacuum degree -0.08MPa, completes acid-base neutralization reaction；
S404. it is depressed in atmosphere at room temperature, starts high-speed stirring apparatus, in the case where revolving speed is 120rpm, 6kg thiosulfuric acid S is added,
S'-1,6- hexylene glycol ester disodium salt switch to stir 1h under 250rpm；
S405. the product in step S404 is placed in vacuum oven, takes out, is cooled to room temperature after dry 5h at 110 DEG C,
The sieve that 100 mesh numbers are crossed after milled processed, is prepared novel cobaltous octadecanate adhesion promotor.
Comparative example:
Novel cobaltous octadecanate adhesion promotor includes following raw material: 150g odium stearate, 32g waterless cobaltous chloride, 4g tripolyphosphate
Sodium, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；
The preparation method of novel cobaltous octadecanate adhesion promotor the following steps are included:
S401. 150g odium stearate is dissolved in the distilled water that 1L temperature is 80 DEG C, preparation obtains aqueous solution of sodium stearate, will
The aqueous solution of sodium stearate be placed at 80 DEG C keep the temperature it is spare；
S402. 32g waterless cobaltous chloride is dissolved in 300mL distilled water, preparation obtains cobalt chloride solution；
S403. the cobalt chloride solution in step S402 is added in the reactor equipped with agitating device, PH meter and heating device,
4g sodium tripolyphosphate is added into reactor, at stirring rate 300r/min, 70 DEG C of heating temperature, with the dropwise addition speed of 5mL/s
Aqueous solution of sodium stearate in step S401 is added in reactor by rate, and during the reaction by the way that quality point is constantly added dropwise
Number makes the pH value of solution in reactor remain at 9.5 for 25% concentrated ammonia liquor, and after being added dropwise, 8g thiosulfuric acid S is added,
S'-1,6- hexylene glycol ester disodium salt stop heating and stirring operation, the mixed system in reactor are filtered, is removed later
Filtrate is gone, flocky precipitate is prepared；
S404. the sediment in step S403 is washed using distilled water, until it can't detect chloride ion；
S405. the sediment in step S404 is placed in vacuum oven, is taken out after dry 7h at 110 DEG C, is cooled to room
Temperature crosses the sieve of 100 mesh numbers after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
Performance test:
One, the physical and chemical index for the novel cobaltous octadecanate adhesion promotor prepared in above-described embodiment and comparative example is tested,
Test result is as follows shown in table 2；Wherein, table 1 is the standard index of cobaltous octadecanate adhesion promotor；
Two, the novel cobaltous octadecanate adhesion promotor prepared in above-described embodiment and comparative example full steel wire is successively fabricated to carry
The belt sizing material of baryon radial tire, all raw material dosages are all consistent in formula system, test sizing material adhesive property and its
Degradation, test result is as follows shown in table 3.
Table 1
| Project | Standard index |
| Appearance | Hyacinthine or aubergine are granular |
| Cobalt mass percent (%) | 9.6±0.6 |
| Softening point (DEG C) | 80~100 |
| Ash content mass percent (550 DEG C) (%) | ≤13.4 |
| Density (g/cm3) | 1.09±0.03 |
| Infrared spectroscopy (reference standard map) | It is comparable |
Table 2
| Project | Embodiment one | Embodiment two | Embodiment three | Example IV | Comparative example |
| Appearance | Aubergine | Aubergine | Aubergine | Aubergine | Aubergine |
| Cobalt content (%) | 6.49 | 6.83 | 6.71 | 6.64 | 9.4 |
| Softening point (DEG C) | 86 | 85 | 86 | 85 | 88 |
| Ash content (550 DEG C) (%) | 11.5 | 11.8 | 12.1 | 11.9 | 12.5 |
| Density (g/cm3) | 1.14 | 1.17 | 1.09 | 1.12 | 1.12 |
| Infrared spectroscopy | It is comparable | It is comparable | It is comparable | It is comparable | It is comparable |
Table 3
| Project | Embodiment one | Embodiment two | Embodiment three | Example IV | Comparative example |
| Tack (N) | 34 | 33 | 34 | 33 | 25 |
| Extraction force (N) | 878 | 861 | 874 | 871 | 764 |
| Extraction force (N) after 100 DEG C × 48h aging | 789 | 796 | 811 | 809 | 673 |
Claims (10)
- The novel cobaltous octadecanate adhesion promotor that 1. a kind of viscosity is strong, cobalt content is low, which is characterized in that including following parts by weight The raw material of proportion: 150 parts of odium stearate, 20.5~24 parts of waterless cobaltous chlorides, 8~11.5 parts of Dehydrated nickel chlorides, 3~4 parts of trimerizations Sodium phosphate, 5~10 parts of thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salts；The preparation method of above-mentioned adhesion promotor makes the following steps are included: by under the dispersion adjustment effect of sodium tripolyphosphate Replace the divalent cobalt ion of a part with bivalent nickel ion, realize modification to cobaltous octadecanate, then with after cure stabilizer Thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt is sufficiently compound, and novel cobaltous octadecanate adhesion promotor is prepared；Or the raw material including following parts by weight proportion: 20 parts of stearic acid, 1865,2.2 parts of cobalt hydroxides, 1 part of nickel hydroxide, 6 Part thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt；Above-mentioned stearic acid, at vacuum degree -0.08MPa, in cobalt hydroxide Divalent cobalt ion and nickel hydroxide in bivalent nickel ion acid-base neutralization reaction directly occurs, generate novel cobaltous octadecanate, then It is sufficiently compound with after cure stabilizer thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt, it is viscous that novel cobaltous octadecanate is prepared Close promotor.
- 2. adhesion promotor according to claim 1, which is characterized in that the adhesion promotor includes following parts by weight The raw material of proportion: 150g odium stearate, 20.5g waterless cobaltous chloride, 11.5g Dehydrated nickel chloride, 3g sodium tripolyphosphate, 10g are thio Sulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
- 3. adhesion promotor according to claim 1, which is characterized in that the adhesion promotor includes following parts by weight The raw material of proportion: 150g odium stearate, 23.5g waterless cobaltous chloride, 8.5g Dehydrated nickel chloride, 3.5g sodium tripolyphosphate, 5g are thio Sulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
- 4. adhesion promotor according to claim 1, which is characterized in that the adhesion promotor includes following parts by weight The raw material of proportion: 150g odium stearate, 24g waterless cobaltous chloride, 8g Dehydrated nickel chloride, 4g sodium tripolyphosphate, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
- 5. adhesion promotor according to claim 1, which is characterized in that the preparation method of the adhesion promotor include with Lower step:S1. 150 parts of odium stearate are dissolved in the distilled water that 1L temperature is 60~90 DEG C, it is water-soluble that preparation obtains odium stearate Liquid, which is placed at 60~90 DEG C keep the temperature it is spare；S2. 20.5~24 parts of waterless cobaltous chlorides are dissolved in 200~300mL distilled water, preparation obtains cobalt chloride solution；S3. 8~11.5 parts of Dehydrated nickel chlorides are dissolved in 100mL distilled water, preparation obtains nickel chloride aqueous solution；S4. the nickel chloride aqueous solution in the cobalt chloride solution and step S3 in step S2 is added and is counted equipped with agitating device, PH In the reactor of heating device, 3~4 parts of sodium tripolyphosphates are added into reactor will be in step S1 under heating stirring Aqueous solution of sodium stearate is added drop-wise in reactor, and during the reaction by the way that the concentrated ammonia liquor that mass fraction is 25% is constantly added dropwise So that the pH value of solution in reactor is remained alkalinity, after being added dropwise, be added 5~10 parts of thiosulfuric acids S, S'-1,6- oneself two Alcohol ester disodium salt stops heating and stirring operation, the mixed system in reactor is filtered later, removes filtrate, preparation Obtain flocky precipitate；S5. the sediment in step S4 is washed using distilled water, until it can't detect chloride ion；S6. the sediment in step S5 is placed in vacuum oven, is taken out after dry 6~8h at 105~120 DEG C, it is cooling To room temperature, the sieve of 100 mesh numbers is crossed after milled processed, novel cobaltous octadecanate adhesion promotor is prepared.
- 6. adhesion promotor according to claim 5, which is characterized in that in the step S4, pass through during the reaction The concentrated ammonia liquor that mass fraction is 25%, which is constantly added dropwise, makes the pH value of solution in reactor remain at 9~10.
- 7. adhesion promotor according to claim 6, which is characterized in that in the step S4, pass through during the reaction The concentrated ammonia liquor that mass fraction is 25%, which is constantly added dropwise, makes the pH value of solution in reactor remain at 9.5.
- 8. adhesion promotor according to claim 7, which is characterized in that in the step S4, in stirring rate 300r/ Min, at 70 DEG C of heating temperature, aqueous solution of sodium stearate is added in reactor with the drop rate of 5mL/s.
- 9. adhesion promotor according to claim 8, which is characterized in that in the step S4, put the precipitate in vacuum In drying box, the dry 7h at 110 DEG C.
- 10. adhesion promotor according to claim 9, which is characterized in that the adhesion promotor includes following parts by weight The raw material of number proportion: 150g odium stearate, 24g waterless cobaltous chloride, 8g Dehydrated nickel chloride, 4g sodium tripolyphosphate, 8g thiosulfuric acid S, S'-1,6- hexylene glycol ester disodium salt.
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