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Preparation and detection methods of lithium aluminum hydride tetrahydrofuran solution

A technology of lithium aluminum hydride and tetrahydrofuran, applied in chemical instruments and methods, various metal hydrides, metal hydrides, etc., to achieve the effect of product quality assurance

Inactive Publication Date: 2018-08-03
庄英俊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention proposes a lithium aluminum hydride tetrahydrofuran solution according to the needs of customers. The invention of lithium aluminum hydride tetrahydrofuran solves the problems of safety in actual production, timeliness in the reaction process, safety in transportation and storage, and product quality. guaranteed

Method used

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  • Preparation and detection methods of lithium aluminum hydride tetrahydrofuran solution
  • Preparation and detection methods of lithium aluminum hydride tetrahydrofuran solution
  • Preparation and detection methods of lithium aluminum hydride tetrahydrofuran solution

Examples

Experimental program
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Embodiment 1

[0041] A preparation method of lithium borohydride tetrahydrofuran solution, comprising the following steps:

[0042] (2) Accurately take by weighing 133g aluminum trichloride and dissolve it in ether for later use;

[0043] (3) Ethyl ether is added in the there-necked flask, then 32g of lithium hydride is added, after stirring evenly, the aluminum chloride solution is slowly added dropwise to the there-necked flask. The total ether consumption is 800g, and the reaction is carried out after adding the initiator , to control the reaction rate,

[0044] (4) After 4.5 hours of reaction time, the precipitation was completed for 5 hours, and then the supernatant was poured out, and the solution was distilled and decompressed to make it into a lithium aluminum hydride solid powder;

[0045] (5) The lithium aluminum hydride solid powder is then dissolved in tetrahydrofuran in proportion to form a lithium aluminum hydride tetrahydrofuran solution.

Embodiment 2-8

[0047] The steps are the same as in Example 1, wherein the amount of reactants and the reaction conditions are shown in Table 1.

Embodiment 9

[0049] Measure the method for lithium aluminum hydride content in the lithium aluminum hydride tetrahydrofuran that embodiment 1-8 makes:

[0050] 1) Take a clean and dry Erlenmeyer flask and weigh it accurately in a ten-thousandth analytical balance;

[0051] 2) Take the sample and put it in the Erlenmeyer flask, seal it with a cap, and accurately weigh to obtain the sample weight W;

[0052] 3) The mixed solution of water and dioxane is added in the constant pressure funnel;

[0053] 4) Connect the constant pressure funnel with the Erlenmeyer flask containing the sample and the gas constant pressure capacity measuring instrument to form a closed system, and make the level of the constant pressure device and the scale tube relative to each other, and accurately record the scale tube in the gas constant pressure capacity measuring instrument volume, denoted as V 1 ;

[0054] 5) Place the Erlenmeyer flask containing the sample in an ice-water bath;

[0055] 6) Add the mixed...

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Abstract

The invention discloses a preparation method of a lithium aluminum hydride tetrahydrofuran solution. The preparation method comprises the steps as follows: (1) lithium hydride is accurately weighed for later use; (2) aluminum trichloride is accurately weighed and dissolved in ether for later use; (3) ether is added to a three-neck flask, lithium hydride is added, after uniform stirring, the aluminum trichloride solution is slowly dropwise added to the three-neck flask, an initiator is added for a reaction, and the reaction temperature is controlled; (4) precipitation is performed for 5 h afterthe reaction, a liquid supernatant is poured out, and the solution is subjected to distillation under reduced pressure to become lithium aluminum hydride solid powder; (5) the lithium aluminum hydride solid powder is dissolved in tetrahydrofuran, and the lithium aluminum hydride tetrahydrofuran solution is formed. The invention also discloses a method for determining the content of lithium aluminum hydride in the lithium aluminum hydride tetrahydrofuran solution. The lithium aluminum hydride prepared with the preparation method is high in active hydrogen content, mild in reaction condition, higher in safety and convenient to use, transport and store.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry, in particular to a preparation method of lithium aluminum hydride tetrahydrofuran solution. Background technique [0002] Lithium aluminum hydride, Chinese alias: Lithium aluminum hydride, molecular formula: LiALH 4 , molecular weight: 37.9543, CAS number: 16853-85-3, lithium aluminum hydride (Lithium Aluminum Hydride) is a complex hydride, white or off-white crystal, is a very important reducing agent in organic synthesis, especially for lipids, carboxylic acids and reduction of amides. Pure lithium aluminum hydride is a white crystalline solid, relatively stable below 120°C and in dry air, but decomposes explosively when exposed to water, its melting point is 140°C, insoluble in hydrocarbons, soluble in ether, tetrahydrofuran, dimethyl solvent Fiber, slightly soluble in n-butyl ether, insoluble or extremely soluble in hydrocarbons and dioxane, its density is relative density (water ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/24G01N7/18
CPCC01B6/243G01N7/18
Inventor 庄英俊
Owner 庄英俊