Method for preparing nontoxic zirconium octoate

Abstract

The invention discloses a method for preparing nontoxic zirconium octoate, comprising the following steps: first throwing octoic acid (RCOOH) into a saponification reactor, then mixing NaOH at a concentration of 30% with the octoic acid (RCOOH) until the pH is 7-8, heating the mixture to the temperature of 70-80 DEG C to undergo saponification reaction for 40min; carrying out synthetic reaction on saponification solution, adding zirconium oxychloride with 10% of saponification solution, a 200<#> solvent with 10% of saponification solution and a 120<#> solvent with 5% of saponification solution in the synthetic reaction, heating to 90-95 DEG C and stirring for 40min; carrying out washing twice after the synthetic reaction, adding a mixed extractant of a P350 extractant [methyl phosphonate di-(1-methylheptyl)] and a P204 extractant di-(2-ethyl phosphonic acid), with mixture ratio of 0.8 to 0.2, and carrying out standing and separating; carrying out reduced pressure distillation on organic phases at a temperature of 180-200 DEG C for 50-60min after separating and dehydrating; regulating zirconium content and filtering to prepare the finished product of zirconium octoate. The method not only features high yield, low cost and mild reaction conditions, but also protects the environment without pollution and can realize industrialized production.

Description

technical field

[0001] The invention relates to a method for preparing zirconium isooctanoate, more specifically relates to a method for preparing non-toxic zirconium isooctanoate, which is suitable for industrial batch production. Background technique

[0002] Zirconium isooctanoate (zirconium 2-ethylhexanoate), English name: Zirconium octoate; Zirconium isooctanoate. Molecular formula: 2(C 8 h 15 o 2 ) ZrO.

[0003] structural formula Yellow-green transparent liquid.

[0004] It is used as a drier for paints and inks. It has unique drier properties, improves the through-drying of paint films and has multifunctionality. It can replace toxic lead drier in paints, so it can be used in lead-free paints; Used as a heat stabilizer for PVC plastics, it can effectively replace toxic lead heat stabilizers, such as tribasic lead sulfate, dibasic lead phosphite, composite lead, lead naphthenate, and lead isooctanoate. It is a product that protects human health and prevents po...

Examples

Embodiment 1

[0031] Example 1: first put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% NaOH and isooctanoic acid (RCOOH) to PH7, heat to 70°C and carry out saponification reaction for 40 minutes; then saponification liquid enters the synthesis reaction , add saponification solution 10% zirconium oxychloride and saponification solution 10% 200 # , saponification solution 5% 120 # Solvent, heat up to 90°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 180° C.; 50 min; the zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

Embodiment 2

[0032] Example 2: First put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% NaOH and isooctanoic acid (RCOOH) to pH 7.5, heat to 75°C for saponification for 40 minutes; then put the saponification solution into Synthesis reaction, add 10% zirconium oxychloride of saponification liquid and 200% of saponification liquid 10% in synthesis reaction # , saponification solution 5% 120 # Solvent, heat up to 93°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 190° C.; 55 minutes; zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

Embodiment 3

[0033] Example 3: first put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% concentration of NaOH and isooctanoic acid (RCOOH) to PH8, heat to 80°C and carry out saponification reaction for 40min; then saponification liquid enters the synthesis reaction , add saponification solution 10% zirconium oxychloride and saponification solution 10% 200 # , saponification solution 5% 120 # Solvent, heat up to 95°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 200° C.; 60 min; zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

[0034] Saponification, according to the requirements of the present invention for the optimal yield to material ratio; h...

technical field

[0001] The invention relates to a method for preparing zirconium isooctanoate, more specifically relates to a method for preparing non-toxic zirconium isooctanoate, which is suitable for industrial batch production. Background technique

[0002] Zirconium isooctanoate (zirconium 2-ethylhexanoate), English name: Zirconium octoate; Zirconium isooctanoate. Molecular formula: 2(C 8 h 15 o 2 ) ZrO.

[0003] structural formula Yellow-green transparent liquid.

[0004] It is used as a drier for paints and inks. It has unique drier properties, improves the through-drying of paint films and has multifunctionality. It can replace toxic lead drier in paints, so it can be used in lead-free paints; Used as a heat stabilizer for PVC plastics, it can effectively replace toxic lead heat stabilizers, such as tribasic lead sulfate, dibasic lead phosphite, composite lead, lead naphthenate, and lead isooctanoate. It is a product that protects human health and prevents po...

Examples

Embodiment 1

[0031] Example 1: first put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% NaOH and isooctanoic acid (RCOOH) to PH7, heat to 70°C and carry out saponification reaction for 40 minutes; then saponification liquid enters the synthesis reaction , add saponification solution 10% zirconium oxychloride and saponification solution 10% 200 # , saponification solution 5% 120 # Solvent, heat up to 90°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 180° C.; 50 min; the zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

Embodiment 2

[0032] Example 2: First put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% NaOH and isooctanoic acid (RCOOH) to pH 7.5, heat to 75°C for saponification for 40 minutes; then put the saponification solution into Synthesis reaction, add 10% zirconium oxychloride of saponification liquid and 200% of saponification liquid 10% in synthesis reaction # , saponification solution 5% 120 # Solvent, heat up to 93°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 190° C.; 55 minutes; zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

Embodiment 3

[0033] Example 3: first put isooctanoic acid (RCOOH) into the saponification tank, then mix 30% concentration of NaOH and isooctanoic acid (RCOOH) to PH8, heat to 80°C and carry out saponification reaction for 40min; then saponification liquid enters the synthesis reaction , add saponification solution 10% zirconium oxychloride and saponification solution 10% 200 # , saponification solution 5% 120 # Solvent, heat up to 95°C, stir, 40min; wash twice with water after synthesis reaction, add P350 extractant [di-(1-methylheptyl methylphosphonate)] and P204 extractant di-(2-ethylhexanoic acid) ) mixed extractant, mixing ratio: 0.8:0.2 standing for separation; the organic phase after separation and dehydration was subjected to vacuum distillation at 200° C.; 60 min; zirconium metal content was adjusted and filtered to obtain the finished zirconium isooctanoate.

[0034] Saponification, according to the requirements of the present invention for the optimal yield to material ratio; h...

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