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Dimeric fatty acid diamine, preparation method and method for preparing dimeric fatty acid diisocyanate

A technology of dimer fatty acid diisocyanate and dimer fatty acid diamine, which is applied in the field of chemical synthesis of materials, can solve problems such as difficult industrial production, and achieve the effect of simple and feasible process, easy implementation and pure product

Inactive Publication Date: 2010-09-29
湖南省方正达电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a higher yield, but it is not easy to realize industrial production due to the unstable intermediate of the dimer fatty acid carbonyl azide, and the DDI obtained by the Cirtius rearrangement method is 36-carbon diisocyanate

Method used

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  • Dimeric fatty acid diamine, preparation method and method for preparing dimeric fatty acid diisocyanate
  • Dimeric fatty acid diamine, preparation method and method for preparing dimeric fatty acid diisocyanate
  • Dimeric fatty acid diamine, preparation method and method for preparing dimeric fatty acid diisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of dimer fatty acid diamine:

[0029] Under ice-salt bath cooling conditions, 60 g of ether reaction medium diethyl ether, 3.7 g of metal hydride reducing agent sodium borohydride and 5.6 g of dimer fatty acid diamide were added into the reaction flask. After mixing, the ice-water bath was removed and replaced with a heating water bath, and the reaction mixture was heated to reflux step by step, and reacted for 30 hours. Extracted 4 times with dichloromethane, using 20g of dichloromethane each time, after the extraction was completed, the extracts were combined.

[0030] The combined extracts were washed twice with water, and the amount of water used for each wash was 20 g. Dry with 5 g of anhydrous sodium sulfate for 3 hours. Then add 5g of active carbon and decolorize for 15 minutes. Finally, methylene chloride was removed by vacuum distillation. The temperature of the vacuum distillation was 40° C., and the vacuum degree was 10 mmHg. After 40 minutes o...

Embodiment 2

[0043] Under cooling in an ice-salt bath, 60 g of tetrahydrofuran, 3.8 g of lithium aluminum hydride, and 5.6 g of dimer fatty acid diamide were added to the reaction flask. After the addition, the ice-water bath was removed and replaced with a heating water bath, and the reaction mixture was heated to reflux step by step, and reacted for 48 hours. Extract with ethylene dichloride 4 times, use 20g ethylene dichloride each time, after the extraction is completed, combine the extracts.

[0044] The combined extracts were washed twice with water, and the amount of water used for each wash was 20 g. Dry with 5 g of anhydrous sodium sulfate for 3 hours. Then add 5g of active carbon and decolorize for 15 minutes. Finally, dichloroethane was removed by vacuum distillation to obtain dimer fatty acid diamine. The vacuum distillation temperature was 50° C., and the vacuum degree was 10 mmHg. After 50 minutes of distillation, no solvent was distilled out, and the distillation was stopp...

Embodiment 3

[0049] Under cooling in an ice-salt bath, 60 g of tetrahydrofuran, 5.3 g of potassium borohydride and 5.6 g of dimer fatty acid diamide were added to the reaction flask. After the addition, the ice-water bath was removed and replaced with a heating water bath, and the reaction mixture was heated to reflux step by step, and reacted for 48 hours. Extract with chloroform 4 times, use 20g chloroform each time, combine extract solution after extraction finishes.

[0050] The combined extracts were washed twice with water, and the amount of water used for each wash was 20 g. Dry with 5 g of anhydrous sodium sulfate for 3 hours. Then add 5g of active carbon and decolorize for 15 minutes. Finally, chloroform was removed by vacuum distillation to obtain dimer fatty acid diamine. The vacuum distillation temperature was 50° C., and the vacuum degree was 10 mmHg. After 50 minutes of distillation, no solvent was distilled out, and the distillation was stopped. A light yellow liquid prod...

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Abstract

The invention discloses a dimeric fatty acid diamine and a preparation method thereof. The invention adopts the dipoly fatty acid diamine as a raw material and provides a method for preparing dimeric fatty acid diisocyanate. The preparation method comprises the steps: by weight, mixing 30-80 parts of ether reaction medium, 4 parts of metal hydride reducing agent and 5 parts of dimeric fatty acid diamide under ice-water bath, carrying out temperature rising, backflow and reaction for 12-50 hours on the obtained reaction mixture, then carrying out treatment of extraction, washing, drying and decoloring and preparing and obtaining the dimeric fatty acid diamine which can be used for carrying out condensation with triphosgene directly and preparing the dimeric fatty acid diisocyanate. The invention prepares the dimeric fatty acid diamine by the reduction of dimeric amide, and has high reaction yield and pure products. The method for directly preparing DDI has mild reaction conditions in the preparation process, simple and feasible technique and easy implementation, and the synthetic method of the products is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of dimer fatty acid diisocyanate (DDI), in particular to a kind of dimer fatty acid diamine (DDAm) as a raw material for synthesizing dimer fatty acid diisocyanate and its preparation method, belonging to the technical field of chemical synthesis of materials . Background technique [0002] Dimeric fatty acid diisocyanate (DDI) is a long carbon chain diisocyanate, the reactivity of the N=C=O functional group in its molecular structure is reduced, and it is an aliphatic diisocyanate with a large molecular weight and low toxicity and a medium reaction rate. [0003] Regarding the application of DDI, a comprehensive review has been found in "Literature Dimeric Fatty Acid Diisocyanates and Their Applications" ([J], Advancing Technology, 1988, 4: 55-61). The application of DDI in hydroxyl-terminated polybutadiene propellants is expected to provide good process performance and excellent mechanical properties, an...

Claims

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Application Information

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IPC IPC(8): C07C211/25C07C209/50C07C265/14C07C263/10
Inventor 李战雄茅沈杰杜丽萍成丽
Owner 湖南省方正达电子科技有限公司
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