Preparation method of lithium 12-hydroxystearate

A technology of lithium dodecyl hydroxystearate and lauryl hydroxystearate, which is applied in the field of preparation of lithium stearate, can solve the problems of high free stearic acid, incomplete reaction of stearate, and low purity, and achieve Low cost, improved product purity, and high yield

Inactive Publication Date: 2018-03-27
GANFENG LITHIUM CO LTD
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Problems solved by technology

The stearate prepared by this type of method has the problems of incomplete reaction, high free stearic acid and low purity
Th

Method used

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  • Preparation method of lithium 12-hydroxystearate
  • Preparation method of lithium 12-hydroxystearate
  • Preparation method of lithium 12-hydroxystearate

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preparation example Construction

[0033] A kind of preparation method of lithium dodecyl hydroxystearate of the present invention, comprises the following steps: comprises the following steps:

[0034] A. Mix dodecyl hydroxystearic acid and water at a ratio of 1:10-1:5, raise the temperature of the prepared raw materials to 90°C-100°C to make lauryl hydroxystearic acid miscible in water, and heat the mixture at 90°C -100°C constant temperature for 40min-60min to obtain dodecyl hydroxystearic acid solution;

[0035] B. Mix lithium hydroxide monohydrate with water to form a lithium hydroxide solution with a mass percent concentration of 2.5%-10%, raise the temperature to 80°C-90°C, and keep the temperature at 80°C-90°C for 15min-30min to obtain hydroxide Lithium solution;

[0036] C, the lithium hydroxide solution obtained in the above-mentioned B step is added to the dodecyl hydroxystearic acid solution obtained in the above-mentioned A step according to the ratio of lithium hydroxide and dodecyl hydroxysteari...

Embodiment 1

[0057] A. Put 50g of dodecyl hydroxystearic acid with a main content of 97.51% in a beaker, add 500g of water, raise the temperature to 90°C to make dodecyl hydroxystearic acid miscible in water, and keep the temperature at 90°C for 60 minutes to obtain dodecyl hydroxystearic acid fatty acid solution.

[0058] B. Take 7.5g of lithium hydroxide monohydrate with a main content of 57.08% in a beaker, add 75g of water to dissolve it in water to form a 5.19% lithium hydroxide solution, raise the temperature to 90°C, and keep the temperature at 90°C for 15 minutes to obtain lithium hydroxide solution.

[0059] C. Add the 90°C mass percentage concentration of 5.19% lithium hydroxide solution prepared in step B to the lauryl hydroxystearic acid solution at 90°C obtained in step A at a molar ratio of 1.1 to carry out neutralization reaction , maintained at 90° C. and stirred for 40 minutes to obtain a reaction liquid.

[0060] D. Emulsifying the reaction liquid obtained in the above ...

Embodiment 2

[0068] A. Take 50g of lauryl hydroxystearic acid with a main content of 97.51% in a beaker, add 300g of water, heat up to 95°C to make lauryl hydroxystearic acid miscible in water, and keep the temperature at 95°C for 50 minutes to obtain lauryl hydroxystearin acid solution.

[0069] B. Take 7.5g of lithium hydroxide monohydrate with a main content of 57.08% in a beaker, add 157.5g of water to dissolve it in water to make a 2.59% lithium hydroxide solution, raise the temperature to 85°C, and keep the temperature at 85°C for 30 minutes until the hydroxide is oxidized lithium solution.

[0070] C. Add the 85°C mass percentage concentration of 2.59% lithium hydroxide solution prepared in step B to the 95°C lauryl hydroxystearic acid solution prepared in step A according to the molar ratio of 1.1 for neutralization reaction, and maintain Stir the reaction at 90° C. for 50 minutes to obtain a reaction liquid.

[0071] D. Emulsifying the reaction liquid obtained in the above step ...

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Abstract

The invention discloses a preparation method of lithium 12-hydroxystearate. The method comprises the following steps: A. mixing 12-hydroxystearic acid with water, then heating up to 90-100 DEG C, andmaintaining the constant temperature for 40-60min to obtain a 12-hydroxystearic acid solution; B. mixing lithium hydroxide monohydrate with water to prepare a lithium hydroxide solution with a concentration of 2.5-10%, heating up to 80-90 DEG C, and maintaining the constant temperature for 15-30min; C. adding the lithium hydroxide solution into the 12-hydroxystearic acid solution, maintaining thetemperature to be 90 DEG C or above, carrying out a neutral reaction, and stirring for carrying out a reaction for 40-60min; D. after the reaction is finished, carrying out an emulsion reaction for 15-30min; E. after emulsification is finished, carrying out centrifugal dewatering, and carrying out elution on the product with hot water at the temperature of 90 DEG C or above until the pH value of the washing liquid is 8-9 so as to obtain a lithium 12-hydroxystearate wet material; F. drying the lithium 12-hydroxystearate wet material to obtain a dry material; G. crushing the dry material to obtain the finished product. The preparation method of the lithium 12-hydroxystearate has the advantages of simple process, , low cost and high yield, can effectively reduce free acid amount in the lithium 12-hydroxystearate finished product, greatly improves the purity of the finished product.

Description

technical field [0001] The invention relates to a method for preparing lithium stearate, in particular to a method for preparing lithium dodecyl hydroxystearate. Background technique [0002] The molecular formula of lithium lauryl hydroxystearate is C 18 h 35 LiO 3 , the structural formula is as follows, the melting point is 202-208 ° C, it is stable at normal temperature and pressure, and insoluble in water, ethanol and ethyl acetate. It has strong thickening ability to mineral oil and synthetic oil. Compared with calcium-based and sodium-based lubricating grease, the amount of thickener can be reduced by about 1 / 3, and the service life can be extended by one to several times. Therefore, it is of great significance to study the production process of lithium lauryl hydroxystearate. [0003] [0004] The method for preparing stearate at present is mainly metathesis method, for example, application number is that 201410756626.5 patent literature discloses a kind of pre...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C59/01
CPCC07C51/412C07C59/01
Inventor 李良彬章小明廖萃许鑫付晓春符龙彭莉娟黄璐璐李芳芳
Owner GANFENG LITHIUM CO LTD
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