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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
adhesion promotor
parts
cobaltous
cobaltous octadecanate
chloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910378984.XA
Other languages
Chinese (zh)
Inventor
孙延亮
邹德鹏
孙永帅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Love Perth Chemical Ltd By Share Ltd
Original Assignee
Dalian Love Perth Chemical Ltd By Share Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian Love Perth Chemical Ltd By Share Ltd filed Critical Dalian Love Perth Chemical Ltd By Share Ltd
Priority to CN201910378984.XA priority Critical patent/CN110055009A/en
Publication of CN110055009A publication Critical patent/CN110055009A/en
Pending legal-status Critical Current

Links

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

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

The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low
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)

  1. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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.
CN201910378984.XA 2019-05-08 2019-05-08 The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low Pending CN110055009A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910378984.XA CN110055009A (en) 2019-05-08 2019-05-08 The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910378984.XA CN110055009A (en) 2019-05-08 2019-05-08 The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low

Publications (1)

Publication Number Publication Date
CN110055009A true CN110055009A (en) 2019-07-26

Family

ID=67322549

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910378984.XA Pending CN110055009A (en) 2019-05-08 2019-05-08 The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low

Country Status (1)

Country Link
CN (1) CN110055009A (en)

Citations (8)

* Cited by examiner, † Cited by third party
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
CN1912040A (en) * 2006-08-24 2007-02-14 朝阳市征和化工有限公司 Composite metal salt adhesion improver and its preparation method
CN102807485A (en) * 2011-06-01 2012-12-05 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
CN103265728A (en) * 2013-06-14 2013-08-28 江苏卡欧化工有限公司 Preparation method of cobalt decanoate adhesion promoter with high performance and low cobalt content
CN103265727A (en) * 2013-06-14 2013-08-28 江苏卡欧化工有限公司 Preparation method of cobalt stearate adhesion promoter with high performance and low cobalt content
JP2014080639A (en) * 2012-10-12 2014-05-08 Nippon Parkerizing Co Ltd Aqueous metal surface treatment agent, metal surface treatment film and metallic material with metal surface treatment film
CN104212410A (en) * 2014-09-11 2014-12-17 北京东方雨虹防水技术股份有限公司 Steel bridge epoxy asphalt waterproof binding material as well as preparation method and application thereof
JP2015227388A (en) * 2014-05-30 2015-12-17 東洋インキＳｃホールディングス株式会社 Adhesive and adhesive sheet

Patent Citations (8)

* Cited by examiner, † Cited by third party
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
CN1912040A (en) * 2006-08-24 2007-02-14 朝阳市征和化工有限公司 Composite metal salt adhesion improver and its preparation method
CN102807485A (en) * 2011-06-01 2012-12-05 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
JP2014080639A (en) * 2012-10-12 2014-05-08 Nippon Parkerizing Co Ltd Aqueous metal surface treatment agent, metal surface treatment film and metallic material with metal surface treatment film
CN103265728A (en) * 2013-06-14 2013-08-28 江苏卡欧化工有限公司 Preparation method of cobalt decanoate adhesion promoter with high performance and low cobalt content
CN103265727A (en) * 2013-06-14 2013-08-28 江苏卡欧化工有限公司 Preparation method of cobalt stearate adhesion promoter with high performance and low cobalt content
JP2015227388A (en) * 2014-05-30 2015-12-17 東洋インキＳｃホールディングス株式会社 Adhesive and adhesive sheet
CN104212410A (en) * 2014-09-11 2014-12-17 北京东方雨虹防水技术股份有限公司 Steel bridge epoxy asphalt waterproof binding material as well as preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
江畹兰等: ""对氨基苯甲酸钴盐及镍盐对天然橡胶与黄铜粘合的增进作用"", 《特种橡胶制品》 *
温辉梁等: "《精细化工产品生产系列 化工助剂》", 31 December 2009, 江西科学技术出版社 *

Similar Documents

Publication Publication Date Title
EP4286325A1 (en) Method for resource recycling of nickel-iron alloy and use thereof
CN102603000B (en) Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material
CN105070903B (en) Ternary positive electrode material precursor, preparation method and application thereof
CN101837958B (en) Preparation method of high temperature stability insoluble sulfur
CN109182791B (en) Method for removing aluminum from rare earth feed liquid by organic acid complexation-solid phase adsorption
CN113234217B (en) Preparation method of solid base catalyst and application of solid base catalyst in continuous production of polyether polyol
CN1322067C (en) Method for producing iron oxide black
CN101864088A (en) Preparation method of compound type cobalt stearate adhesion promoter
CN110055009A (en) The novel cobaltous octadecanate adhesion promotor that a kind of viscosity is strong, cobalt content is low
CN102838561A (en) Production method of rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide)
CN101462942A (en) Method for producing high purity battery level iron oxalate from pickle liquor
CN114276817A (en) Soil repairing agent and preparation method and application thereof
CN103435081B (en) Method for producing low-iron limestone
CN101972708A (en) Preparation method of feldspar ore reverse-flotation de-ironing collector
CN110041851A (en) The novel new cobalt decanoate adhesion promotor that a kind of viscosity is strong, cobalt content is low
CN108129290B (en) Method for removing sulfate radical in lactic acid
CN110092942A (en) A kind of novel cobaltous octadecanate adhesion promotor and preparation method improving cobalt content
CN115709979A (en) Method for preparing battery-grade manganese iron phosphate by taking high-iron manganese ore as raw material
CN101602516A (en) The preparation method of aluminum fluoride
CN108912328A (en) A kind of preparation method of heavy metal ion chelating agent
CN103569971B (en) Boiling roaster nickel-molybdenum ore prepares the method for sulfuric acid
CN103007899A (en) Preparation method of heavy metal ion absorption resin
CN109384872B (en) Chelate resin and preparation method and application thereof
CN105646962A (en) Corrosion-resistant rubber
CN107140861B (en) Method for producing cement retarder by using fresh phosphogypsum

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20190726

RJ01 Rejection of invention patent application after publication