CN116655463A - Preparation method of aqueous drier cobalt iso-octoate - Google Patents
Preparation method of aqueous drier cobalt iso-octoate Download PDFInfo
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- CN116655463A CN116655463A CN202310646191.8A CN202310646191A CN116655463A CN 116655463 A CN116655463 A CN 116655463A CN 202310646191 A CN202310646191 A CN 202310646191A CN 116655463 A CN116655463 A CN 116655463A
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- octoate
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- 239000010941 cobalt Substances 0.000 title claims abstract description 82
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 82
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 30
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229940044175 cobalt sulfate Drugs 0.000 claims abstract description 21
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims abstract description 21
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 11
- 238000007127 saponification reaction Methods 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims description 68
- 229920005989 resin Polymers 0.000 claims description 68
- 238000001179 sorption measurement Methods 0.000 claims description 43
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 34
- SAXJVKAVLPPFLI-UHFFFAOYSA-N prop-2-enoic acid;1,1,3,3-tetramethylguanidine Chemical compound OC(=O)C=C.CN(C)C(=N)N(C)C SAXJVKAVLPPFLI-UHFFFAOYSA-N 0.000 claims description 22
- 239000012074 organic phase Substances 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 20
- 239000003456 ion exchange resin Substances 0.000 claims description 17
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 17
- -1 primary amino ion exchange resin Chemical compound 0.000 claims description 17
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- YJBLTYRYUXKJLE-UHFFFAOYSA-N 3-amino-1h-quinoline-4-thione Chemical compound C1=CC=C2C(=S)C(N)=CNC2=C1 YJBLTYRYUXKJLE-UHFFFAOYSA-N 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 229910001410 inorganic ion Inorganic materials 0.000 claims description 9
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 8
- MMEDJBFVJUFIDD-UHFFFAOYSA-N 2-[2-(carboxymethyl)phenyl]acetic acid Chemical compound OC(=O)CC1=CC=CC=C1CC(O)=O MMEDJBFVJUFIDD-UHFFFAOYSA-N 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 8
- IRBDRMFJBYHCEO-UHFFFAOYSA-L cobalt(2+);prop-2-enoate Chemical compound [Co+2].[O-]C(=O)C=C.[O-]C(=O)C=C IRBDRMFJBYHCEO-UHFFFAOYSA-L 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000000717 retained effect Effects 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000003957 anion exchange resin Substances 0.000 claims description 2
- 239000013065 commercial product Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013067 intermediate product Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000006184 cosolvent Substances 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 description 2
- INJAHHABQHQOMY-UHFFFAOYSA-N 2-(dihydroxymethyl)butanoic acid Chemical compound CCC(C(O)O)C(O)=O INJAHHABQHQOMY-UHFFFAOYSA-N 0.000 description 2
- PSJBSUHYCGQTHZ-UHFFFAOYSA-N 3-Methoxy-1,2-propanediol Chemical compound COCC(O)CO PSJBSUHYCGQTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- KXZSVYHFYHTNBI-UHFFFAOYSA-N 1h-quinoline-2-thione Chemical compound C1=CC=CC2=NC(S)=CC=C21 KXZSVYHFYHTNBI-UHFFFAOYSA-N 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-M 2-ethylhexanoate Chemical compound CCCCC(CC)C([O-])=O OBETXYAYXDNJHR-UHFFFAOYSA-M 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-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
- 229910012988 LiCo3 Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- SHZIWNPUGXLXDT-UHFFFAOYSA-N caproic acid ethyl ester Natural products CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- 238000003926 complexometric titration Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- XHCCWBJFZUXJBV-UHFFFAOYSA-K trisodium 2-[(2-oxido-5-sulfophenyl)diazenyl]-3,6-disulfonaphthalene-1,8-diolate Chemical compound C1=CC(=C(C=C1S(=O)(=O)O)N=NC2=C(C3=C(C=C(C=C3C=C2S(=O)(=O)O)S(=O)(=O)O)[O-])[O-])[O-].[Na+].[Na+].[Na+] XHCCWBJFZUXJBV-UHFFFAOYSA-K 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The application relates to the field of fine chemical industry, in particular to a preparation method of an aqueous drier cobalt iso-octoate; the method adopts isooctanoic acid, water, sodium hydroxide solution, solvent oil and cobalt sulfate feed liquid, and after saponification and double decomposition reaction, the mixture is stood for layering, washed by hot water, distilled and concentrated to obtain aqueous drier cobalt isooctanoate; the application adopts NaOH precipitation method to recycle Co in water phase 2+ The utilization rate of the metal cobalt can be effectively improved; because the isooctanoic acid has good solubility and purityThe water-based drier cobalt iso-octoate prepared by the method has the characteristics of high quality, light color, no peculiar smell and the like, and has the advantages of good miscibility, light color, high cobalt content and the like; the aqueous drier cobalt iso-octoate prepared by the application is used in the coating, so that the coating is colorless and transparent, does not yellow, has low viscosity and greatly improves the quality of the coating.
Description
Technical Field
The application relates to the field of fine chemical industry, in particular to a preparation method of an aqueous drier cobalt iso-octoate.
Background
Cobalt iso-octoate, also called as 2-ethyl hexanoate, is an organic compound with a chemical formula of C16H30CoO4, and is mainly used as a drier for paint and ink, a curing accelerator for unsaturated polyester resin, a polyvinyl chloride stabilizer, a polymerization catalyst and the like; used as an accelerator for curing unsaturated polyester adhesives, etc.
A method for preparing cobalt iso-octoate by utilizing waste lithium battery positive electrode lithium cobaltate (patent number CN 200910013221.1), which uses waste lithium battery positive electrode lithium cobaltate powder; acidolysis is carried out by adopting a chemical extraction and stripping method, fe and Al are removed by chemical precipitation, filter pressing is carried out to remove residues, a self-made auxiliary extractant is added to P204 to remove impurities, a self-made auxiliary extractant is added to P507 to extract and separate Co, li and other procedures, so that cobalt sulfate Coso4 liquid with the content of 75-80% is prepared, and the primary deposition rate of lithium carbonate LiCo3 is more than 75% by raffinate deposition. The cobalt sulfate solution and sodium isooctanoate obtained after saponification of isooctanoic acid and sodium hydroxide are subjected to double decomposition reaction, and the cobalt isooctanoate liquid product is obtained after washing, standing delamination, dehydration, metal content adjustment and filtration. The recovery rate of cobalt in the lithium cobalt oxide powder of the positive electrode of the waste lithium battery is more than 97 percent.
A waterborne oxidative crosslinking resin drier and a preparation method thereof (patent number: CN 202111417988.8) are provided, wherein dimethylolbutyric acid, water and a cosolvent are utilized to prepare a dimethylolbutyric acid solution; taking a dihydroxymethyl butyric acid solution, adding powdery cobalt hydroxide, reacting, filtering, testing the cobalt metal content in the filtrate, and supplementing water or cosolvent to make the cobalt content be 4-4.5 wt%, thus obtaining an intermediate product 1; dripping a solution of a metal activity promoter into the intermediate product 1, and stirring to obtain an intermediate product 2; taking a dihydroxymethyl butyric acid solution, adding water and a cosolvent, adding powdery zirconium carbonate and lithium hydroxide, reacting, testing the metal content, and adding water or the cosolvent to ensure that the metal content is 3.5-4wt% to prepare an intermediate product 3; and mixing the intermediate product 2 and the intermediate product 3, and stirring at normal temperature to obtain the water-based oxidative crosslinking resin drier. The waterborne oxidative crosslinked resin drier is easy to add, good in water resistance, good in drier property and strong in universality, and the production process is clean.
The water-base alkyd resin is prepared through multi-step reaction with vegetable oleic acid, polyol except glycerol monomethyl ether, glycerol monomethyl ether and polybasic acid or anhydride as reaction material and water-carrying agent as reflux solvent. The water-based alkyd resin has improved water resistance and adhesive force, and the method realizes the reutilization of the glycerol and improves the utilization value of the glycerol.
However, the applicant believes that the preparation methods of cobalt iso-octoate in the above patents and the prior art mainly comprise a melting method, a direct method, an ammonia method and the like; but these methods exist: high investment, high cost, complex process flow, harsh reaction conditions, low yield, low utilization rate of metallic cobalt and the like.
Disclosure of Invention
In order to solve at least one technical problem in the preparation of the cobalt iso-octoate, the application aims to provide a preparation method of the aqueous drier cobalt iso-octoate, which can effectively improve the utilization rate of metallic cobalt, and the prepared aqueous drier cobalt iso-octoate is used in a coating, so that the coating is colorless and transparent, does not yellow, has low viscosity and greatly improves the quality of the coating.
The technical scheme of the application is as follows:
according to one aspect of the application, the application discloses a preparation method of an aqueous drier cobalt iso-octoate, which comprises the following operation steps:
s1: weighing 20-30 parts of isooctanoic acid and 30-60 parts of water according to parts by weight, adding into a reaction kettle, heating to 60-90 ℃, and stirring;
s2: adding 18-30 parts of sodium hydroxide solution, stirring, and performing saponification reaction for 20-45min;
s3: then continuously adding 60-80 parts of solvent oil, uniformly stirring, slowly dropwise adding 5-15 parts of cobalt sulfate feed liquid, and carrying out double decomposition reaction for 40-70min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
Further, the stirring speed is 300-800rpm.
Further, the mass concentration of the sodium hydroxide solution is 10-15%.
Further, the solvent oil is 70#, 90#, 120#, 180#, 190#, 200#, 260#.
Further, the mass concentration of the cobalt sulfate feed liquid is 10-30%.
Further, the distillation temperature is controlled between 180 ℃ and 220 ℃.
According to a second aspect of the present application, the present application discloses a method for adsorption by using an adsorption resin through a column, which mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 20-30% of the volume of the exchange column;
step 2: controlling the flow rate to be 1-3BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 45-55 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
Further, the preparation method of the adsorption resin comprises the following steps:
s1: adding 70-100 parts of primary amino ion exchange resin and 500-1000 parts of DMF (dimethyl formamide) into a three-port reaction bottle according to parts by weight, and stirring for 2-4 hours;
s2: adding 0.01-0.3 part of cobalt acrylate, 1-3 parts of sodium methoxide, 0.01-0.1 part of 3-amino-4-mercaptoquinoline, and reacting for 20-50 minutes at 50-60 ℃; then adding 5-10 parts of tetramethylguanidine acrylate, and reacting for 120-150 minutes at 50-60 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
Further, the primary amino ion exchange resin is a commercial product, and is a weak basic anion exchange resin (R-NH 2), such as 701 type resin.
Further, the preparation method of the tetramethylguanidine acrylate comprises the following steps:
110-150 parts of tetramethylguanidine and 70-100 parts of acrylic acid are added into a reaction kettle, and stirred for 30-50 minutes at 50-65 ℃ to prepare tetramethylguanidine acrylate.
Reaction mechanism:
according to the application, primary amino ion exchange resin and cobalt acrylate, 3-amino-4-mercapto quinoline and tetramethyl guanidine acrylate respectively undergo amino addition reaction to obtain adsorption resin containing cobalt ions on a framework and tetramethyl guanidine and mercapto quinoline, so that the compatibility with cobalt isooctanoate and the adsorption capacity to impurities can be provided, and the purity of cobalt isooctanoate is improved.
The technical effects are as follows:
compared with the prior art, the preparation method of the aqueous drier cobalt iso-octoate has the following remarkable effects:
1. the application adopts NaOH precipitation method to recycle Co in water phase 2+ The utilization rate of the metal cobalt can be effectively improved;
2. the cobalt iso-octoate has the characteristics of good solubility, high purity, stable quality, light color, no peculiar smell and the like, so that the aqueous drier cobalt iso-octoate prepared by the application has the advantages of good miscibility, light color, high cobalt content and the like;
3. the aqueous drier cobalt iso-octoate prepared by the application is used in the coating, so that the coating is colorless and transparent, does not yellow, has low viscosity and greatly improves the quality of the coating.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described in the following in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments.
In the specific embodiment of the application, the cobalt content in the water phase and the discharged water is determined by adopting an atomic absorption spectrophotometry analysis. Volume of the organic phase after water washing was measured 1mL and placed in a 250mL Erlenmeyer flask. However, the method is thatThen adding 20-30 mL absolute ethyl alcohol to dissolve the organic phase, and shaking uniformly. Accurately adding 25 mLETTA standard solution, adding 10mL ammonia water-ammonium chloride buffer solution, controlling pH to about 10, adding 3-4 drops of acid chrome blue K as indicator, and using ZnCl 2 Back titration is performed on the standard titration solution, and the end point is the moment when the solution changes from blue to pink. Thus, the cobalt content in the organic phase can be analyzed by complexometric titration.
The indexes such as gloss, hardness and the like of the liquid paint drier are detected according to the specified standard of ANSI/ASTMD600-73 in the United states.
Example 1
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 20g of isooctanoic acid and 30g of water, adding into a reaction kettle, heating to 60 ℃, and stirring;
s2: adding 18g of sodium hydroxide solution, stirring, and performing saponification reaction for 20min;
s3: then 60g of solvent oil is continuously added, the mixture is stirred uniformly, 5g of cobalt sulfate feed liquid is slowly added dropwise, and the double decomposition reaction is carried out for 40min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 300rpm.
The mass concentration of the sodium hydroxide solution is 10%.
The solvent oil is 70#.
The mass concentration of the cobalt sulfate feed liquid is 10%.
The distillation temperature is controlled at 180 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 20% of the volume of the exchange column;
step 2: controlling the flow rate to be 1BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 45 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 70g of primary amino ion exchange resin and 500g of DMF are added into a three-port reaction bottle, and stirred for 2h;
s2: 0.01g of cobalt acrylate, 1g of sodium methoxide, 0.01g of 3-amino-4-mercaptoquinoline and the reaction time at 50℃for 20 minutes; then 5g of tetramethylguanidine acrylate is added for reaction for 120 minutes at 50 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
The preparation method of the tetramethylguanidine acrylate comprises the following steps:
110g of tetramethylguanidine, 70g of acrylic acid was added to the reaction vessel and stirred at 50℃for 30 minutes to prepare tetramethylguanidine acrylate.
Example 2
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 24g of isooctanoic acid and 40g of water, adding into a reaction kettle, heating to 70 ℃, and stirring;
s2: adding 22g of sodium hydroxide solution, stirring, and performing saponification reaction for 30min;
s3: then continuously adding 65g of solvent oil, uniformly stirring, slowly dripping 8g of cobalt sulfate feed liquid, and carrying out double decomposition reaction for 50min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 400rpm.
The mass concentration of the sodium hydroxide solution is 10%.
The solvent oil is 90#.
The mass concentration of the cobalt sulfate feed liquid is 20%.
The distillation temperature is controlled at 190 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 25% of the volume of the exchange column;
step 2: controlling the flow rate to be 2BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 50 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 80g of primary amino ion exchange resin and 600g of DMF are added into a three-port reaction bottle, and stirred for 3 hours;
s2: 0.1g of cobalt acrylate, 2g of sodium methoxide, 0.05g of 3-amino-4-mercaptoquinoline are added and reacted for 30 minutes at 55 ℃; 7g of tetramethylguanidine acrylate is added and reacted for 130 minutes at 55 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
The preparation method of the tetramethylguanidine acrylate comprises the following steps:
120g of tetramethylguanidine, 80g of acrylic acid was added to the reaction vessel and stirred at 55℃for 35 minutes to prepare tetramethylguanidine acrylate.
Example 3
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: 28g of isooctanoic acid and 50g of water are weighed, added into a reaction kettle, heated to 80 ℃ and stirred;
s2: 26g of sodium hydroxide solution is added, stirred and saponified for 40min;
s3: then continuously adding 75g of solvent oil, uniformly stirring, slowly dripping 13g of cobalt sulfate feed liquid, and carrying out double decomposition reaction for 60min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 700rpm.
The mass concentration of the sodium hydroxide solution is 15%.
The solvent oil is 120#.
The mass concentration of the cobalt sulfate feed liquid is 20%.
The distillation temperature is controlled at 210 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 25% of the volume of the exchange column;
step 2: controlling the flow rate to be 2BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 50 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 90g of primary amino ion exchange resin and 900g of DMF are added into a three-port reaction bottle and stirred for 3 hours;
s2: 0.2g of cobalt acrylate, 2g of sodium methoxide, 0.08g of 3-amino-4-mercaptoquinoline are added and reacted for 40 minutes at 55 ℃; 9g of tetramethylguanidine acrylate is added and reacted for 140 minutes at 55 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
The preparation method of the tetramethylguanidine acrylate comprises the following steps:
140g of tetramethylguanidine, 90g of acrylic acid was added to the reaction vessel and stirred at 60℃for 45 minutes to prepare tetramethylguanidine acrylate.
Example 4
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 30g of isooctanoic acid and 60g of water, adding into a reaction kettle, heating to 90 ℃, and stirring;
s2: adding 30g of sodium hydroxide solution, stirring, and performing saponification reaction for 45min;
s3: then continuously adding 80g of solvent oil, uniformly stirring, slowly dripping 15g of cobalt sulfate feed liquid, and carrying out double decomposition reaction for 70min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 800rpm.
The mass concentration of the sodium hydroxide solution is 15%.
The solvent oil is 260#.
The mass concentration of the cobalt sulfate feed liquid is 30%.
The distillation temperature is controlled at 220 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 30% of the volume of the exchange column;
step 2: controlling the flow rate to be 3BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 55 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 100g of primary amino ion exchange resin and 1000g of DMF are added into a three-port reaction bottle and stirred for 4 hours;
s2: 0.3g of cobalt acrylate, 3g of sodium methoxide, 0.1g of 3-amino-4-mercaptoquinoline are added and reacted for 50 minutes at 60 ℃; then 10g of tetramethylguanidine acrylate is added and reacted for 150 minutes at 60 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
The preparation method of the tetramethylguanidine acrylate comprises the following steps:
150g of tetramethylguanidine, 100g of acrylic acid was added to the reaction vessel and stirred at 65℃for 50 minutes to prepare tetramethylguanidine acrylate.
Comparative example 1
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 20g of isooctanoic acid and 30g of water, adding into a reaction kettle, heating to 60 ℃, and stirring;
s2: adding 18g of sodium hydroxide solution, stirring, and performing saponification reaction for 20min;
s3: then 60g of solvent oil is continuously added, the mixture is stirred uniformly, 5g of cobalt sulfate feed liquid is slowly added dropwise, and the double decomposition reaction is carried out for 40min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 300rpm.
The mass concentration of the sodium hydroxide solution is 10%.
The solvent oil is 70#.
The mass concentration of the cobalt sulfate feed liquid is 10%.
The distillation temperature is controlled at 180 ℃.
Comparative example 2
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 20g of isooctanoic acid and 30g of water, adding into a reaction kettle, heating to 60 ℃, and stirring;
s2: adding 18g of sodium hydroxide solution, stirring, and performing saponification reaction for 20min;
s3: then 60g of solvent oil is continuously added, the mixture is stirred uniformly, 5g of cobalt sulfate feed liquid is slowly added dropwise, and the double decomposition reaction is carried out for 40min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 300rpm.
The mass concentration of the sodium hydroxide solution is 10%.
The solvent oil is 70#.
The mass concentration of the cobalt sulfate feed liquid is 10%.
The distillation temperature is controlled at 180 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 20% of the volume of the exchange column;
step 2: controlling the flow rate to be 1BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 45 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 70g of primary amino ion exchange resin and 500g of DMF are added into a three-port reaction bottle, and stirred for 2h;
s2: 1g of sodium methoxide and 0.01g of 3-amino-4-mercaptoquinoline are added and reacted for 20 minutes at 50 ℃; then 5g of tetramethylguanidine acrylate is added for reaction for 120 minutes at 50 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
The preparation method of the tetramethylguanidine acrylate comprises the following steps:
110g of tetramethylguanidine, 70g of acrylic acid was added to the reaction vessel and stirred at 50℃for 30 minutes to prepare tetramethylguanidine acrylate.
Comparative example 3
The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 20g of isooctanoic acid and 30g of water, adding into a reaction kettle, heating to 60 ℃, and stirring;
s2: adding 18g of sodium hydroxide solution, stirring, and performing saponification reaction for 20min;
s3: then 60g of solvent oil is continuously added, the mixture is stirred uniformly, 5g of cobalt sulfate feed liquid is slowly added dropwise, and the double decomposition reaction is carried out for 40min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
The stirring speed was 300rpm.
The mass concentration of the sodium hydroxide solution is 10%.
The solvent oil is 70#.
The mass concentration of the cobalt sulfate feed liquid is 10%.
The distillation temperature is controlled at 180 ℃.
The method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 20% of the volume of the exchange column;
step 2: controlling the flow rate to be 1BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 45 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
The preparation method of the adsorption resin comprises the following steps:
s1: 70g of primary amino ion exchange resin and 500g of DMF are added into a three-port reaction bottle, and stirred for 2h;
s2: 0.01g of cobalt acrylate, 1g of sodium methoxide, 0.01g of 3-amino-4-mercaptoquinoline and the reaction time at 50℃for 20 minutes; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
The primary amino ion exchange resin is 701 type resin.
| Conversion/% | Gloss/% | Hardness of | |
| Example 1 | 95.98 | 94 | 0.69 |
| Example 2 | 96.32 | 95 | 0.73 |
| Example 3 | 96.63 | 96 | 0.77 |
| Example 4 | 96.57 | 95 | 0.75 |
| Comparative example 1 | 83.91 | 85 | 0.25 |
| Comparative example 2 | 90.13 | 91 | 0.63 |
| Comparative example 3 | 91.22 | 93 | 0.65 |
The foregoing describes specific embodiments of the present application. It is to be understood that the application is not limited to the particular embodiments described above, and that various changes or modifications may be made by those skilled in the art within the scope of the appended claims without affecting the spirit of the application. The embodiments of the application and the features of the embodiments may be combined with each other arbitrarily without conflict.
Claims (10)
1. The preparation process of water-base drier cobalt isooctanoate includes the following steps:
s1: weighing 20-30 parts of isooctanoic acid and 30-60 parts of water according to parts by weight, adding into a reaction kettle, heating to 60-90 ℃, and stirring;
s2: adding 18-30 parts of sodium hydroxide solution, stirring, and performing saponification reaction for 20-45min;
s3: then continuously adding 60-80 parts of solvent oil, uniformly stirring, slowly dropwise adding 5-15 parts of cobalt sulfate feed liquid, and carrying out double decomposition reaction for 40-70min;
s4: after the reaction, standing for layering, washing the upper layer liquid with hot water for 3 times, and removing SO in the organic phase 4 2－ An inorganic ion;
s5: and (3) distilling the washed organic phase at normal pressure, and then adsorbing by using an adsorption resin through a column to obtain the aqueous drier cobalt iso-octoate.
2. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the stirring speed is 300-800rpm.
3. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the mass concentration of the sodium hydroxide solution is 10-15%.
4. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the solvent oil is 70#, 90#, 120#, 180#, 190#, 200#, 260#.
5. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the mass concentration of the cobalt sulfate feed liquid is 10-30%.
6. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the distillation temperature is controlled between 180 ℃ and 220 ℃.
7. The method for preparing the aqueous drier cobalt iso-octoate according to claim 1, which is characterized in that: the method for adsorbing by using the adsorption resin through the column mainly comprises the following steps:
step 1: flowing the organic dissimilar cobalt octoate washed by the S4 into a exchange column with a certain capacity, wherein the resin addition amount is 20-30% of the volume of the exchange column;
step 2: controlling the flow rate to be 1-3BV/h, slowly flowing cobalt iso-octoate into an exchange column where the adsorption resin is positioned, and controlling the temperature to be 45-55 ℃;
step 3: the impurities adsorbed by the adsorption resin are retained in the column, and the purified cobalt iso-octoate is collected at the other end of the exchange column, so that the purified cobalt iso-octoate is obtained.
8. The method for preparing the aqueous drier cobalt iso-octoate according to claim 7, which is characterized in that: the preparation method of the adsorption resin comprises the following steps:
s1: adding 70-100 parts of primary amino ion exchange resin and 500-1000 parts of DMF (dimethyl formamide) into a three-port reaction bottle according to parts by weight, and stirring for 2-4 hours;
s2: adding 0.01-0.3 part of cobalt acrylate, 1-3 parts of sodium methoxide, 0.01-0.1 part of 3-amino-4-mercaptoquinoline, and reacting for 20-50 minutes at 50-60 ℃; then adding 5-10 parts of tetramethylguanidine acrylate, and reacting for 120-150 minutes at 50-60 ℃; filtering, and vacuum drying to constant weight to obtain the adsorbent resin.
9. The method for preparing the aqueous drier cobalt iso-octoate according to claim 8, which is characterized in that: the primary amino ion exchange resin is a commercial product and is a weak alkaline anion exchange resin (R-NH 2), such as 701 type resin.
10. The method for preparing the aqueous drier cobalt iso-octoate according to claim 8, which is characterized in that: the preparation method of the tetramethylguanidine acrylate comprises the following steps:
110-150 parts of tetramethylguanidine and 70-100 parts of acrylic acid are added into a reaction kettle, and stirred for 30-50 minutes at 50-65 ℃ to prepare tetramethylguanidine acrylate.
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| CN116273194A (en) * | 2023-03-25 | 2023-06-23 | 江苏可奥熙光学材料科技有限公司 | Novel catalyst for resin monomer with refractive index of 1.56 |
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