A kind of method for salting out of trimethyl borate

A trimethyl borate and salting-out technology, which is applied in the field of mixture analysis and purification, can solve the problems of high cost, cumbersome operation, and long time consumption, and achieve the effects of high yield, simple process, and avoiding strict requirements

Inactive Publication Date: 2017-01-18
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in the present invention is to overcome the disadvantages of complex operation, long time consumption and high cost during the salting out of trimethyl borate in the prior art, and provide a method for salting out of trimethyl borate with low cost, simple and fast

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  • A kind of method for salting out of trimethyl borate

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Effect test

Embodiment 1

[0052] Weigh 2.0g of 20-80 mesh mixed mesh powder calcium chloride in a 100ml iodine measuring bottle; mix the azeotrope composed of trimethyl borate and methanol with the calcium chloride evenly, wherein trimethyl borate The mass ratio of ester to methanol is 70%: 30%; the above mixture is oscillated, wherein the oscillating ambient temperature is 20°C, the oscillating time is 10min, and the oscillating speed is 280r / min to obtain the first oscillating liquid; The liquid is transferred to a separatory funnel, and separated after standing for 30 minutes. The upper layer is a trimethyl borate layer, and the lower layer is a salt and alcohol layer. The upper layer and the lower layer are titrated to analyze the purity of trimethyl borate. The purity of trimethyl borate in the upper layer is 91.64 And the yield is 83.12, the quality of the lower layer is 12.9, which contains 36.90% of trimethyl borate.

Embodiment 2

[0054] Weigh 4.0g of 20-80 mesh mixed mesh powder calcium chloride in a 100ml iodine measuring bottle; mix the azeotrope composed of trimethyl borate and methanol with the calcium chloride evenly, wherein trimethyl borate The mass ratio of ester to methanol is 70%: 30%, wherein the ambient temperature of oscillation is 30°C, the oscillation time is 20min, and the oscillation speed is 300r / min to obtain the first oscillation liquid; Liquid funnel, separate liquid after standing for 30 minutes, the upper layer is a trimethyl borate layer, the lower layer is a salt and alcohol layer, take the upper layer and the lower layer to titrate and analyze the purity of trimethyl borate, the upper layer trimethyl borate has a purity of 93.40 and a yield of 89.30, The lower mass 13.2 contains trimethyl borate 23.11%.

Embodiment 3

[0056] Weigh 1.0g of 20-80 mesh mixed mesh powder calcium chloride in a 100ml iodine measuring bottle, and mix the azeotrope composed of trimethyl borate and methanol with the calcium chloride evenly, wherein trimethyl borate The mass ratio of ester to methanol is 70%: 30%, wherein, the ambient temperature of oscillation is 30°C, the oscillation time is 30min, and the oscillation speed is 320r / min to obtain the first oscillation liquid; the first oscillation liquid is static, and Obtain the upper liquid of the first oscillating liquid to obtain the trimethyl borate layer, wherein the resting time is 20 min; add the trimethyl borate layer to the calcium chloride for oscillation to obtain the second oscillating liquid, Among them, the oscillation is under the same conditions as the first oscillation; the second oscillation liquid is transferred to the separatory funnel, and the oscillation is over. Since the solution is no longer stratified, suction filtration is selected, and it...

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Abstract

The invention provides a salting-out method of trimethyl borate. The method comprises the following steps: uniformly mixing an azeotrope formed by trimethyl borate and methanol with calcium chloride; then, oscillating the mixture to obtain a first oscillating liquid; and standing the first oscillating liquid and obtaining the supernatant liquid of the first oscillating liquid to obtain the trimethyl borate layer. The salting-out method of trimethyl borate provided by the invention salts out at normal pressure to obtain high purity trimethyl borate, so that a plant byproduct calcium chloride is fully utilized to avoid strict demand on equipment by sulfuric acid. Furthermore, the method is simple in technical process, high in yield, green and environment-friendly and easy to realize production on a large scale.

Description

[0001] 【Technical field】 [0002] The invention relates to the technical field of mixture analysis and purification, in particular to a method for salting out trimethyl borate. [0003] 【Background technique】 [0004] Trimethyl borate (B(CH 3 O) 3 ) is one of the organic borates with important uses. Trimethyl borate was used as a solvent, plasticizer, catalyst, welding flux and flame retardant in the early days. Due to the development of science and technology and the needs of industrial development, trimethyl borate is currently used in high-grade borate esters, high-purity boron The preparation and synthesis of borohydride compounds have important applications. As a raw material for hydrogen storage materials, it can be used to manufacture high-energy fuels and hydrogen source fuel cells, and is a new energy raw material. [0005] At present, the methods for purifying trimethyl borate include: adding salt method, adding alkali metal or alkaline earth metal alcoholate meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/04
Inventor 李海民党亚侯殿保吴辉陈育刚孟瑞英杨海云
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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