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A method for decomposing ammonium chloride and simultaneously preparing organic base hydrochloride and cyclohexanone oxime

A technology of organic base hydrochloride and cyclohexanone oxime, which is applied in the field of chemical technology, can solve the problems of harsh reaction conditions, unfavorable industrialization, expensive displacers, etc., and achieve the effect of convenient transportation

Inactive Publication Date: 2017-08-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The displacer of this method is expensive, the reaction conditions are harsh, and it is not conducive to industrialization (Zeng Fengchun, Inorganic Salt Industry, 2009, 41 (9): 1-3)

Method used

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  • A method for decomposing ammonium chloride and simultaneously preparing organic base hydrochloride and cyclohexanone oxime
  • A method for decomposing ammonium chloride and simultaneously preparing organic base hydrochloride and cyclohexanone oxime
  • A method for decomposing ammonium chloride and simultaneously preparing organic base hydrochloride and cyclohexanone oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 3.0g of TS-1 titanium silicon catalyst and 8.0g (150mmol) of ammonium chloride solid into the reactor, then add water 20mL (1111.1mmol), cyclohexylamine 17.2mL (150mmol), cyclohexanone 6.4mL (62mmol ), stirred and warmed up to 70°C, then added 20mL of hydrogen peroxide (H 2 o 2 196mmol), the hydrogen peroxide is added dropwise and injected by a micro-injection pump, 20mL / h (dropping is completed in 1 hour), and the normal pressure reaction is started for 1.5h at the same time; the catalyst and the reaction solution are centrifuged, and the catalyst obtained is washed with alcohol and water, and the 80 ℃ vacuum drying for 10 hours, 500 ℃ muffle furnace roasting for 4 hours, and set aside; the reaction solution obtained by centrifugation was extracted and separated by toluene to obtain an organic phase, and the organic phase was analyzed by gas chromatography, and the yield of the product cyclohexanone oxime was quantitatively calculated to be 86.1 %; The above organ...

Embodiment 2～7

[0038] The operation steps and reaction conditions are the same as in Example 1, except that cyclohexylamine is replaced by other organic bases, which are respectively dimethylamine, trimethylamine, diethylamine, triethylamine, ethylenediamine, and ethanolamine. is 150mmol. The organic phase was analyzed by gas chromatography, the yield of the product cyclohexanone oxime and the quality of organic base hydrochloride were quantitatively calculated, and various organic base hydrochloride products were characterized by infrared. The experimental results are shown in Table 1, and the characterization results are attached Figure 2-7 .

[0039] The impact of different organic bases in table 1 on the reaction of synthetic cyclohexanone oxime

[0040]

[0041]

Embodiment 8

[0043] The same operation steps and reaction conditions as in Example 1, except that in the oximation reaction, the addition of cyclohexylamine was changed to 7.6mL, and the amount of cyclohexylamine was 66mmol. After the reaction was over, the catalyst and the reaction solution were centrifuged. The organic phase is obtained through toluene extraction and separation, and the organic phase composition is analyzed by gas chromatography; the raffinate aqueous phase is distilled under reduced pressure, washed and dried to obtain the white solid cyclohexylamine hydrochloride crude product 12.2g (which contains 4.1g ammonium chloride ). The experimental results are shown in Table 2.

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Abstract

The invention discloses a method for decomposing ammonium chloride to prepare organic base hydrochloride and cyclohexanone-oxime synchronously. The method comprises the steps of placing a titanium silicalite molecular sieve based catalyst and ammonium chloride solid in a reactor, adding organic base and cyclohexanone, conducting stirring, increasing temperature to 40-90 DEG C, and adding hydrogen peroxide solution dropwise for normal-pressure reaction lasting 1-6 h; conducting centrifugal separation on the catalyst and reaction solution, conducting extraction separation on reaction solution obtained after centrifugal separation so that an organic phase can be obtained, and conducting reduced pressure distillation on the organic phase so that the white solid cyclohexanone-oxime product can be obtained; conducting reduced pressure distillation on raffinate, and then conducting washing and drying so that organic base hydrochloride can be obtained, wherein organic base is cyclohexylamine, dimethylamine, trimethylamine, diethylamine, triethylamine, ethylenediamine or ethanol amine. Through the catalytic reaction process for direct synthesis of cyclohexanone-oxime and organic base hydrochloride, N and Cl in ammonium chloride molecules are utilized at the same time.

Description

technical field [0001] The invention relates to a novel method for preparing organic alkali hydrochloride and cyclohexanone oxime by simultaneously utilizing chlorine and nitrogen elements in ammonium chloride, which belongs to the technical field of chemical technology. Background technique [0002] Ammonium chloride (chemical formula: NH 4 Cl), referred to as "ammonium chloride", also known as halogen sand, colorless crystal or white crystalline powder. Ammonium chloride can be obtained by the neutralization reaction of ammonia gas and hydrogen chloride, or ammonia water and hydrochloric acid. In industry, the soda ash (Na 2 CO 3 ) process, a large amount of ammonium chloride (NH 4 Cl). Among them, a part of ammonium chloride is used as nitrogen fertilizer for agricultural production, while most of the remaining ammonium chloride has no suitable outlet, so that "flooding" has become a bottleneck restricting the sustainable development of the soda ash industry. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/04C07C251/44C07C209/68C07C211/35C07C211/04C07C211/05C07C211/10C07C215/08
CPCC07C209/68C07C249/04C07C251/44C07C211/35C07C211/04C07C211/05C07C211/10C07C215/08
Inventor 王延吉徐元媛张东升李志会孔令凯王淑芳赵新强
Owner HEBEI UNIV OF TECH
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