CN111518477A - Preparation method of efficient drier - Google Patents
Preparation method of efficient drier Download PDFInfo
- Publication number
- CN111518477A CN111518477A CN202010448970.3A CN202010448970A CN111518477A CN 111518477 A CN111518477 A CN 111518477A CN 202010448970 A CN202010448970 A CN 202010448970A CN 111518477 A CN111518477 A CN 111518477A
- Authority
- CN
- China
- Prior art keywords
- isooctanoic acid
- amount
- organic phase
- water
- acid
- 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.)
- Withdrawn
Links
- 238000002360 preparation method Methods 0.000 title claims description 7
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims abstract description 93
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 9
- 239000010941 cobalt Substances 0.000 claims abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 9
- -1 rare earth isooctanoate Chemical class 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 7
- 239000001110 calcium chloride Substances 0.000 claims abstract description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 6
- LSKJZEDMESDBLU-UHFFFAOYSA-L manganese(2+);6-methylheptanoate Chemical compound [Mn+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O LSKJZEDMESDBLU-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 239000012074 organic phase Substances 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 32
- 239000002253 acid Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000007127 saponification reaction Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 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 abstract description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 abstract description 3
- 229940044175 cobalt sulfate Drugs 0.000 abstract description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 239000011734 sodium Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- 229920000180 alkyd Polymers 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- YPIFGDQKSSMYHQ-UHFFFAOYSA-N 7,7-dimethyloctanoic acid Chemical compound CC(C)(C)CCCCCC(O)=O YPIFGDQKSSMYHQ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000003446 ligand Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000005609 naphthenate group Chemical group 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 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
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F9/00—Compounds to be used as driers, i.e. siccatives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The method takes isooctanoic acid as a main raw material, firstly isooctanoic acid reacts with sodium hydroxide solution to generate sodium isooctanoate, and further reacts with cobalt sulfate, manganese sulfate, anhydrous calcium chloride, rare earth and zirconium oxychloride respectively to generate cobalt isooctanoate, manganese isooctanoate, calcium isooctanoate, rare earth isooctanoate and zirconium isooctanoate; and compounding the five carboxylates according to a certain optimized proportion to obtain the efficient drier. The invention not only improves the surface drying speed of the initial drier, but also recycles the waste materials and reduces the cost.
Description
Technical Field
The invention relates to the technical field of paint driers, in particular to a preparation method of an efficient drier.
Background
In the early 20 s of the 19 th century, metal naphthenate was the first drier in modern sense. Currently, the anionic portion of the siccatives used is composed primarily of organic synthetic acids, such as naphthenic acid, isooctanoic acid, and neodecanoic acid. The carboxyl group of isooctanoic acid is attached to a highly branched carbon atom, because the highly branched carboxylate facilitates high solubility of the drier in film-forming materials in non-polar environments, and prevents precipitation of the drier complex due to chemical reactions, thus novel driers have also been developed in high solids and waterborne alkyd coatings.
The drier is one of the most used assistants in paint industry, and is mainly used for oil paint, alkyd paint and alkyd ready-mixed paint containing unsaturated bonds. The drier is generally a soap salt of an alkaline earth metal or a heavy metal, and in order to achieve good dispersion, the anion or ligand part of the drier needs to be miscible with the film-forming material and the solvent. The customary siccatives are carboxylic metal soaps formed from metal cations and carboxylic compounds, which are simple dicarboxylic acid complexes, the metal ion portion of the siccative being present mostly in the form of a plus divalent radical. Because the anionic portion of the siccative determines to a large extent whether the siccative is suitable for use as a siccative, it is desirable that the anionic portion of the siccative have good compatibility and stability in various coating systems and be capable of forming high concentrations with metal ions, and that the formed siccative be of good storage stability, low viscosity, high catalytic efficiency and high cost performance. The high-efficiency novel drier is more and more concerned by people.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an efficient drier which has low production cost and high additional value and can reduce the timeliness of drying, and the specific scheme is as follows:
the preparation method of the efficient drier is characterized by comprising the following steps:
step 1, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the water in a water bath heating condition to 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CoSO4Reacting the feed liquid for 1-1.5 h at the temperature of 95-98 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a cobalt iso-octoate product with the content of 10%;
step 2, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and heating the isooctanoic acid in a water bath to 50 toStirring evenly at 60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding MnSO4Reacting the feed liquid for 1-1.5 h at the temperature of 90-92 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a manganese isooctoate product with the content of 8%;
step 3, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid in a water bath heating mode at 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CaCl2Reacting the feed liquid at the temperature of 90-92 ℃ for 1.0-1.5 h; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a calcium isooctoate product with the content of 5%;
step 4, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid in a water bath heating mode at 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, slowly dropwise adding rare earth feed liquid, and reacting for 1-1.5 h at 82-85 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a rare earth isooctanoate product with the content of 12%;
step 5, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid into a 250 mL three-neck flask, and supplementingAdding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the mixture under the condition of heating the mixture in a water bath to 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of 200 # solvent oil, fully shaking up, and slowly dropwise adding Cl2OZr, reacting the feed liquid for 1-1.5 h at the temperature of 80-82 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a zirconium isooctoate product with the content of 12%;
and 6, adding a proper amount of cobalt isooctanoate in the step 1, manganese isooctanoate in the step 2, calcium isooctanoate in the step 3, rare earth isooctanoate in the step 4 and zirconium isooctanoate in the step 5 into a compound mixing tank, and stirring for 30-45 min at the temperature of 25-30 ℃ to obtain the required efficient drier.
Compared with the prior art, the invention has outstanding substantive characteristics and remarkable progress, and particularly has the following advantages:
the method takes isooctanoic acid as a main raw material, firstly isooctanoic acid reacts with sodium hydroxide solution to generate sodium isooctanoate, and further reacts with cobalt sulfate, manganese sulfate, anhydrous calcium chloride, rare earth and zirconium oxychloride respectively to generate cobalt isooctanoate, manganese isooctanoate, calcium isooctanoate, rare earth isooctanoate and zirconium isooctanoate; and compounding the five carboxylates according to a certain optimized proportion to obtain the efficient drier. The invention not only improves the surface drying speed of the initial drier, but also recycles the waste materials and reduces the production cost.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1:
the preparation method of the efficient drier is characterized by comprising the following steps:
step 1, measuring a certain amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, and supplementing water until the isooctanoic acid2 times of the amount of the mixture, and uniformly stirring the mixture under the condition of heating the mixture to 55 ℃ in a water bath; adding NaOH solution according to 95% (mol percent) of acid amount, stirring at constant temperature for saponification for 0.6 h; then adding a certain amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CoSO4Reacting the feed liquid for 1.2h at the temperature of 95 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 3 times, and then distilling and concentrating to obtain a cobalt isooctanoate product with the content of 10 percent;
step 2, measuring a certain amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid under the condition of heating in a water bath to 50 ℃; adding NaOH solution according to 95% (mol percent) of acid amount, stirring at constant temperature for saponification for 0.8 h; then adding a certain amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding MnSO4Reacting the feed liquid for 1.5 hours at the temperature of 90 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 3 times, and then distilling and concentrating to obtain a manganese isooctoate product with the content of 8 percent;
step 3, measuring a certain amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid under the condition of heating in a water bath to 50 ℃; adding NaOH solution according to 95% (mol percent) of acid amount, stirring at constant temperature for saponification for 0.7 h; then adding a certain amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CaCl2Reacting the feed liquid for 1.2h at the temperature of 92 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, the organic phase is washed by water with the volume of 40 ℃ which is half of the volume of the organic phase, the operation is repeated for 3 times, and then the product of calcium isooctanoate with the content of 5 percent is prepared by distillation and concentration;
step 4, measuring a certain amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid under the condition of heating in a water bath to 50 ℃; adding NaOH solution according to 95% (mol percent) of acid amount, stirring at constant temperature for saponification for 1.0 h; then adding a certain amount of No. 200 solvent oil, fully shaking up, slowly dropwise adding rare earth feed liquid, and reacting for 1.5h at 85 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 3 times, and then distilling and concentrating to obtain a rare earth isooctanoate product with the content of 12 percent;
step 5, measuring a certain amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid under the condition of heating in a water bath to 50 ℃; adding NaOH solution according to 95% (mol percent) of acid amount, stirring at constant temperature for saponification for 0.8 h; then adding a certain amount of No. 200 solvent oil, fully shaking up, and slowly dripping Cl2OZr reacting at 80 deg.C for 1.0 h; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 2 times, and then distilling and concentrating to obtain a zirconium isooctoate product with the content of 12%;
and 6, adding a proper amount of cobalt isooctoate obtained in the step 1, manganese isooctoate obtained in the step 2, calcium isooctoate obtained in the step 3, rare earth isooctoate obtained in the step 4 and zirconium isooctoate obtained in the step 5 into a compound mixing tank, and stirring for 30min at the temperature of 30 ℃ to obtain the required efficient drier.
The method takes isooctanoic acid as a main raw material, firstly isooctanoic acid reacts with sodium hydroxide solution to generate sodium isooctanoate, and further reacts with cobalt sulfate, manganese sulfate, anhydrous calcium chloride, rare earth and zirconium oxychloride respectively to generate cobalt isooctanoate, manganese isooctanoate, calcium isooctanoate, rare earth isooctanoate and zirconium isooctanoate; and compounding the five carboxylates according to a certain optimized proportion to obtain the efficient drier. The invention can not only improve the surface drying speed of the initial drier, but also recycle the waste materials and reduce the cost.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (1)
1. The preparation method of the efficient drier is characterized by comprising the following steps:
step 1, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the water in a water bath heating condition to 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CoSO4Reacting the feed liquid for 1-1.5 h at the temperature of 95-98 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a cobalt iso-octoate product with the content of 10%;
step 2, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the water in a water bath heating condition to 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding MnSO4Reacting the feed liquid for 1-1.5 h at the temperature of 90-92 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then washing the organic phase by adopting water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 2-3 times, and then distilling, concentrating to prepare the productObtaining manganese isooctoate with the content of 8 percent;
step 3, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid in a water bath heating mode at 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, and slowly dropwise adding CaCl2Reacting the feed liquid at the temperature of 90-92 ℃ for 1.0-1.5 h; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using water with the volume of 40 ℃ which is half of the volume of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a calcium isooctoate product with the content of 5%;
step 4, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the isooctanoic acid in a water bath heating mode at 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of No. 200 solvent oil, fully shaking up, slowly dropwise adding rare earth feed liquid, and reacting for 1-1.5 h at 82-85 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; then, washing the organic phase by using 40 ℃ water with the volume being half of the amount of the organic phase, repeatedly operating for 2-3 times, and then distilling and concentrating to obtain a rare earth isooctanoate product with the content of 12%;
step 5, measuring a proper amount of isooctanoic acid, placing the isooctanoic acid in a 250 mL three-neck flask, adding water to 2 times of the amount of the isooctanoic acid, and uniformly stirring the isooctanoic acid and the water in a water bath heating condition to 50-60 ℃; adding NaOH solution according to 95% (mol percentage) of acid amount, stirring at constant temperature for saponification for 0.5-1.0 h; then adding a proper amount of 200 # solvent oil, fully shaking up, and slowly dropwise adding Cl2OZr, reacting the feed liquid for 1-1.5 h at the temperature of 80-82 ℃; transferring the liquid into a 250 mL separating funnel, standing and layering to obtain an upper layer liquid as an organic phase, then carrying out liquid separation operation, and pouring the upper layer liquid into a 150mL beaker; the organic phase is then washed with 40 ℃ water in a volume of half the amount of the organic phaseRepeatedly operating for 2-3 times, and then distilling and concentrating to obtain a zirconium isooctoate product with the content of 12%;
and 6, adding a proper amount of cobalt isooctanoate in the step 1, manganese isooctanoate in the step 2, calcium isooctanoate in the step 3, rare earth isooctanoate in the step 4 and zirconium isooctanoate in the step 5 into a compound mixing tank, and stirring for 30-45 min at the temperature of 25-30 ℃ to obtain the required efficient drier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010448970.3A CN111518477A (en) | 2020-05-25 | 2020-05-25 | Preparation method of efficient drier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010448970.3A CN111518477A (en) | 2020-05-25 | 2020-05-25 | Preparation method of efficient drier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111518477A true CN111518477A (en) | 2020-08-11 |
Family
ID=71908206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010448970.3A Withdrawn CN111518477A (en) | 2020-05-25 | 2020-05-25 | Preparation method of efficient drier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111518477A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122046A (en) * | 2021-04-27 | 2021-07-16 | 中山市富日印刷材料有限公司 | High-gloss quick-drying non-skinning printing ink and preparation method thereof |
| CN113582833A (en) * | 2021-08-27 | 2021-11-02 | 南京晶典抗氧化技术研究院有限公司 | Synthesis method of manganese isooctanoate and preparation method of ink drier |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709334A (en) * | 2013-12-27 | 2014-04-09 | 青岛乐化科技有限公司 | Preparation method of alkyd-acrylate hybrid emulsion |
| CN104893519A (en) * | 2015-05-11 | 2015-09-09 | 广德加点化工有限公司 | Modified aqueous alkyd resin coating |
| CN107760106A (en) * | 2016-08-19 | 2018-03-06 | 中钞油墨有限公司 | Dark ink with multiple anti-fake function |
| CN108424682A (en) * | 2018-04-25 | 2018-08-21 | 安徽以利达罐业有限公司 | A kind of tinplate tin printing ink |
-
2020
- 2020-05-25 CN CN202010448970.3A patent/CN111518477A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709334A (en) * | 2013-12-27 | 2014-04-09 | 青岛乐化科技有限公司 | Preparation method of alkyd-acrylate hybrid emulsion |
| CN104893519A (en) * | 2015-05-11 | 2015-09-09 | 广德加点化工有限公司 | Modified aqueous alkyd resin coating |
| CN107760106A (en) * | 2016-08-19 | 2018-03-06 | 中钞油墨有限公司 | Dark ink with multiple anti-fake function |
| CN108424682A (en) * | 2018-04-25 | 2018-08-21 | 安徽以利达罐业有限公司 | A kind of tinplate tin printing ink |
Non-Patent Citations (3)
| Title |
|---|
| 俞志明: "《中国化工商品大全 1995年版 第3卷》", 31 January 1996, 中国物资出版社 * |
| 涂料工艺编委会: "《涂料工艺》", 31 December 1997, 化学工业出版社 * |
| 黄可龙: "《重有色金属精细化工产品生产技术》", 31 December 1996, 中南工业大学出版 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122046A (en) * | 2021-04-27 | 2021-07-16 | 中山市富日印刷材料有限公司 | High-gloss quick-drying non-skinning printing ink and preparation method thereof |
| CN113122046B (en) * | 2021-04-27 | 2022-06-28 | 中山市富日印刷材料有限公司 | High-gloss quick-drying non-skinning printing ink and preparation method thereof |
| CN113582833A (en) * | 2021-08-27 | 2021-11-02 | 南京晶典抗氧化技术研究院有限公司 | Synthesis method of manganese isooctanoate and preparation method of ink drier |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111518477A (en) | Preparation method of efficient drier | |
| JPH0226635B2 (en) | ||
| CN113603580B (en) | Method for synthesizing methacrylic acid by decarboxylation of itaconic acid | |
| CN102671702A (en) | Method for preparing zinc oxide ionic bond grafting and coordination supported tetra(4-carboxyl phenyl) metalloporphyrin catalyst | |
| CN104211931B (en) | A kind of pure plant oil based polyenoid class UV-curable prepolymer | |
| CN111410916A (en) | Preparation method of drier in white paint | |
| CN110818573B (en) | Preparation method of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane | |
| CN1317255C (en) | Method for synthesizing high-recovery and high-optical purity L-butyl lactate | |
| JPS62108838A (en) | Production of vanadium-containing mixed metal soap solution | |
| CN111574356A (en) | Preparation method of chromium acetate hexahydrate | |
| CN114920648B (en) | Synthesis method and catalyst of 3- (3-oxo-2-amyl) cyclopentyl dimethyl malonate | |
| CN111500195A (en) | Preparation method of drier for preventing surface skinning | |
| US3723152A (en) | Drying oil compositions cobalt drier compositions therefor and process of making same | |
| CN113200937B (en) | Method for preparing 1,2-benzisothiazolin-3-one by catalytic oxidation | |
| CN111484802A (en) | Preparation method of low-cost efficient drier | |
| CN1059198C (en) | Method for one-step manufacture of stannous caprylate | |
| CN1060668A (en) | A kind of production method of rare-earth coatings drier | |
| Bieleman | Driers | |
| CN1287137A (en) | Oxidation process for producing quinacridineone pigment | |
| CN106831399B (en) | Synthetic method of 2-ethylhexanoic acid rhodium (II) | |
| CN1055717C (en) | Method for producing rare earth drier | |
| CN110330428B (en) | Method for preparing diisobutyl phthalate | |
| CN105944762A (en) | Phenanthroline copper complex catalyst, preparation method and application thereof | |
| US4723024A (en) | Preparation of silver carboxylates | |
| CN113582833A (en) | Synthesis method of manganese isooctanoate and preparation method of ink drier |
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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200811 |
|
| WW01 | Invention patent application withdrawn after publication |