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Preparation method of bis (octadecyl) hydroxylamine

A technology of octadecyl and substituted octadecane, which is applied in the field of preparation of bis(octadecyl)hydroxylamine, can solve problems such as lack of research reports, achieve the effect of wide source of raw materials, simple reaction and operation, and meet market demand

Pending Publication Date: 2021-11-16
宿迁盛瑞新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, the use of the hydroxylamine antioxidant bis(octadecyl)hydroxylamine is completely dependent on imports, and related research reports at home and abroad are extremely scarce, and the production process is almost monopolized by foreign countries, forming technical barriers

Method used

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  • Preparation method of bis (octadecyl) hydroxylamine
  • Preparation method of bis (octadecyl) hydroxylamine
  • Preparation method of bis (octadecyl) hydroxylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 1000mL four-neck flask equipped with a thermometer, add 10.4g of hydroxylamine hydrochloride, 120g of triethylamine, and 450g of tetrahydrofuran, install a stirrer and a condenser, and pre-mix for 30 minutes at 30°C. Then, the temperature was raised to 60° C. and 99.9 g of bromooctadecane was added dropwise. After the dropwise addition, the temperature was raised to 85° C. and kept for reaction for 14 hours. After the reaction is finished, the reaction solution is cooled and suction filtered, and the filter cake obtained by suction filtration is washed with water and dried to obtain bis(octadecyl)hydroxylamine as a white powder product.

[0033] The target product prepared in this embodiment is detected by an infrared spectrometer, and the infrared spectrum is as follows: figure 1 shown by figure 1 The infrared spectrum shown can be seen at 1400~1420cm -1 There is a strong carbon-hydrogen bond stretching vibration absorption peak, indicating the presence of v-C-N...

Embodiment 2

[0037] In a 500mL four-neck flask equipped with a thermometer, add 6.94g of hydroxylamine hydrochloride, 84.8g of triethylamine, and 300g of tetrahydrofuran, install a stirrer and a condenser tube, and premix and react at 30°C for 30 minutes. Then, the temperature was raised to 65° C. and 99.9 g of bromooctadecane was added dropwise. After the dropwise addition, the temperature was raised to 87° C. and kept for reaction for 18 hours. After the reaction is finished, the reaction solution is cooled and suction filtered, and the filter cake obtained by suction filtration is washed with water and dried to obtain bis(octadecyl)hydroxylamine as a white powder product.

[0038] The target product prepared in this embodiment is detected by NMR, 1HNMR (400MHz, D O): 2.71 (t, 2H), 2.63 (t, 2H), 1.63 (m, 2H), 1.33 (m, 2H), 1.31 (s, 60H), 0.93 (t, 6H). HNMR spectrum such as figure 2 shown.

Embodiment 3

[0040] In a 500mL four-neck flask equipped with a thermometer, add 8.34g of hydroxylamine hydrochloride, 141.6g of triethylamine, and 300g of tetrahydrofuran, install a stirrer and a condenser, and pre-mix for 30 minutes at 30°C. Then, the temperature was raised to 65° C. and 66.6 g of bromooctadecane and 32.8 g of iodooctadecane were added dropwise. After the dropwise addition, the temperature was raised to 87° C. and kept for reaction for 16 hours. After the reaction is finished, the reaction solution is cooled and suction filtered, and the filter cake obtained by suction filtration is washed with water and dried to obtain bis(octadecyl)hydroxylamine as a white powder product.

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Abstract

The invention relates to a preparation method of bis (octadecyl) hydroxylamine. The method comprises the following steps: adding a raw material solvent, hydroxylamine hydrochloride, an acid-binding agent and a catalyst into a reaction kettle, stirring and pre-mixing, after pre-mixing, heating to a dropwise adding temperature, dropwise adding halogenated octadecane, and then heating to carry out heat preservation reaction; and after the reaction is finished, washing and filtering the reaction liquid, and finally synthesizing the target product bis (octadecyl) hydroxylamine. Halogenated octadecane and hydroxylamine hydrochloride react to generate the product, the catalyst promotes the reaction, the raw materials are wide in source and low in price, the final yield of the product is high, and the method is an ideal process for achieving industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of bis(octadecyl)hydroxylamine. Background technique [0002] At present, the demand for antioxidants at home and abroad is suddenly increasing. The Asia-Pacific region is the region with the largest consumption of antioxidants in the world, accounting for more than 30%, followed by China, accounting for more than 20%. Antioxidants on the market are tending to discolor under the influence of nitrogen oxides, a phenomenon known as gas fading. Decolorization is aggravated by various factors, such as the presence of phenolic antioxidants, the use of phenolic type additives, etc. In inhibiting gas fading and discoloration, hydroxylamine antioxidants avoid the existence of phenolic substances, so that the product has good anti-gas yellowing ability and good color stability, which is more effective than traditional hindered phenolic antioxid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C291/04
CPCC07C291/04
Inventor 刘恩静陈超胡新利王光腾张朋李国华韩炎
Owner 宿迁盛瑞新材料有限公司