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Method for preparing zinc oleate

A technology of zinc oleate and oleic acid is applied in the preparation of carboxylates, carboxylates, organic compounds and other directions, which can solve the problems of easy oxidation of products, large amount of n-hexane, and difficulty in recycling, and avoid oxidation. , the effect of high reaction yield and simple process

Inactive Publication Date: 2019-01-22
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process of this method, the product is easily oxidized, and the amount of n-hexane used is large and difficult to recycle.

Method used

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  • Method for preparing zinc oleate

Examples

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Effect test

preparation example Construction

[0022] The preparation method of zinc oleate of the present invention adopts figure 1 The preparation device shown is carried out, and preparation device comprises a three-necked flask 110, a constant pressure funnel 120, a distillation ball 130, a condensation tube 140 and a ventilation device (not shown on the figure), constant pressure funnel 120 and distillation The balls 130 are respectively inserted into an opening of the three-necked flask 110 for connection, and the condenser tube 140 is inserted into the upper port of the distillation ball 130 for fixed connection.

[0023] The three-neck flask 110 includes a first opening 111, a second opening 112, and a third opening 113, and the third opening 113 is sealed with a bottle stopper.

[0024] The constant pressure funnel 120 is inserted into the first opening 111 and fixedly connected.

[0025] Distillation ball 130 comprises a steam channel 131, a liquid channel 132, a return port 133, a discharge port 134, a changeov...

Embodiment 1

[0036] Take 300g of oleic acid and 120g of zinc acetate into the reaction device, replace the air in the reaction device with nitrogen, turn the switch 135 until the return port 133 is unblocked, reflux at 100°C for 4 hours under stirring conditions, and then turn the changeover switch 135 to the discharge port 134 to be unblocked , steam out acetic acid and discharge from outlet 134, obtain acetic acid 164g altogether, take out the residual acetic acid in the three-necked flask 110 with aeration device, cool to 50 ℃, add 4200g n-hexane in the three-necked flask 110, cool down after fully dissolving, oil The crude zinc oleate product was separated out; the crude zinc oleate product was filtered and washed with water to remove the residual zinc acetate, and then the oleic acid in the crude zinc oleate product was washed away with n-hexane or acetone, followed by vacuum drying to obtain 303 g of zinc oleate finished product.

Embodiment 2

[0038] Take 200g of oleic acid and 90g of zinc acetate into the reaction device, replace the air in the reaction device with nitrogen, turn the switch 135 until the return port 133 is unblocked, reflux at 100°C for 4 hours under stirring conditions, and then turn the changeover switch 135 to the discharge port 134 to be unblocked , steam out the acetic acid and discharge it from the discharge port 134 to obtain 30 g of acetic acid altogether, extract the residual acetic acid in the three-necked flask 110 with a ventilation device, cool to 80° C., add 580 g of n-hexane in the three-necked flask 110, cool down after fully dissolving, oil The zinc oleate crude product is separated out; filter and wash the zinc oleate crude product to remove the zinc acetate remaining therein, then wash off the oleic acid in the zinc oleate crude product with n-hexane or acetone, and then vacuum dry to obtain 176g of zinc oleate finished product.

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Abstract

The invention relates to a method for preparing zinc oleate. The method comprises the following steps: S1, adding zinc acetate and oleic acid in a molar ratio of 1: (1-3) into a reaction unit; S2, replacing air in the reaction unit with protective gas; S3, performing refluxing at 100-180 DEG C for 1-4 h; S4, distilling off acetic acid; S5, extracting residual acetic acid in the reaction unit, carrying out cooling to 50-100 DEG C, adding n-hexane into the reaction unit, performing cooling after sufficient dissolving, and allowing a crude zinc oleate product to be precipitated; S6, subjecting the crude zinc oleate product to filtering and washing so as to remove residual zinc acetate in the crude zinc oleate product, then washing away oleic acid in the crude zinc oleate product by using n-hexane or acetone, and then performing vacuum drying to obtain a finished zinc oleate product. The preparation method for the zinc oleate in the invention adopts the protective gas for protection so asto avoid the oxidation of oleic acid and zinc oleate in a high-temperature reaction process; most of the acetic acid can be separated and recovered as a by-product, and n-hexane and the like can alsobe recycled and reused; and the method is high in reaction yield, simple in process and easy to achieve industrial production.

Description

technical field [0001] The invention relates to the field of preparation of metal organic substances, in particular to a preparation method of zinc oleate. Background technique [0002] Zinc oleate is an important chemical raw material, which can be used to make active additives, catalysts, deodorants, anti-corrosion coatings, and can also be used in composite materials, nanomaterial synthesis and other fields. [0003] At present, there are few reports on the preparation of zinc oleate. Zhang Luyuan used zinc chloride and sodium oleate to synthesize zinc oleate in his doctoral thesis "Synthesis and Properties of ZnO Nanomaterials", and added ethanol, deionized water, and n-hexane Carry out reflux, separate the upper layer solution after reflux, wash with hot water, and obtain zinc oleate after drying. In the preparation process of this method, the product is easily oxidized, and the amount of n-hexane used is large and difficult to recover. [0004] Therefore, it is neces...

Claims

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Application Information

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IPC IPC(8): C07C57/12C07C51/41
CPCC07C51/412C07C57/12
Inventor 马永博朱刘薄福丽
Owner FIRST RARE MATERIALS CO LTD
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