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Preparation method for alkyl alcohol amine

A technology of alkanolamine and alkylamine, which is applied in the field of preparation of alkanolamine, can solve problems such as increasing the difficulty of water separation, reducing the utilization rate of alkylene oxide, and hydrolysis loss of alkylene oxide, and achieving the conversion rate of raw materials and Effects of high recovery, high reactivity and selectivity, and shortened process flow

Active Publication Date: 2015-11-25
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to the excessive amount of amine, after the reaction is completed, a large amount of alkylamine remains, and it is necessary to add a deamination device in the production process to recover the excess alkylamine, so that the entire production process is extended; at the same time, due to the addition of water, A dehydration device is also required, and the presence of water also causes the hydrolysis loss of alkylene oxide and reduces the utilization rate of alkylene oxide; for some special alkanolamines such as N, N-dimethylisopropanolamine, etc. Azeotropes are formed, which will inevitably further increase the difficulty of water separation and also increase the production process
Although there are also patents referring to the method of anhydrous continuous synthesis of alkanolamine products such as patent CN102557960A, etc., these methods still require the recovery process of excess amine

Method used

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  • Preparation method for alkyl alcohol amine
  • Preparation method for alkyl alcohol amine
  • Preparation method for alkyl alcohol amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Add 105g of DEA and 45g of dimethylamine into the reaction kettle. After stirring evenly, add PO in four times with an interval of 10 minutes each time. A total of 63.8g of PO is added. After 3 hours, the material was discharged, and samples were taken for gas chromatography analysis. The conversion rate of dimethylamine was 95.2%, the yield of N,N-dimethylisopropanolamine was 94.4%, and the crude product color 4APHA was synthesized.

[0036] 2. Carry out continuous rectification of the crude product, the vacuum degree is -0.099MPa, the feed temperature is 100°C, the tower top cut-off temperature is 53°C, the purity of the refined N,N-dimethylisopropanolamine product is ≥99.5%, and the color The chromaticity is 0 APHA, the chromaticity is 6 APHA after 90 days at room temperature, and the chromaticity is 50 APHA after 7 days at 60°C.

[0037] 3. After the materials in the rectification column are passed into the reactor, analyze the amount of remaining DEA, add PO aga...

Embodiment 2

[0039] 1. Add 105g of DEA and 45g of dimethylamine into the reaction kettle. After stirring evenly, add PO in five times on average, with an interval of 8 minutes between each time, and a total of 92.8g of PO. Control the reaction temperature at 80°C, and the reaction pressure at 0.7MPa. After 2 hours, the material was discharged, and samples were taken for gas chromatography analysis. The conversion rate of dimethylamine was 99.2%, the yield of N,N-dimethylisopropanolamine was 98.9%, and the crude product color 6APHA was synthesized.

[0040] 2. Carry out continuous rectification of the crude product, the vacuum degree is -0.099MPa, the feed temperature is 100°C, the tower top cut-off temperature is 53°C, the purity of the refined N,N-dimethylisopropanolamine product is ≥99.5%, and the color The color is 0APHA, the color is 4APHA after being placed at room temperature for 90 days, and the color is 57APHA after being placed at 60°C for seven days.

[0041] 3. After the materials...

Embodiment 3

[0043] 1. Add 105g of DEA and 45g of dimethylamine into the reaction kettle. After stirring evenly, add PO in five times on average, with an interval of 7 minutes between each time. A total of 104.4g of PO is added. The reaction temperature is controlled at 60°C, and the reaction pressure is 0.7MPa. After 3 hours, the material was discharged, and samples were taken for gas chromatography analysis. The conversion rate of dimethylamine was 98.7%, the yield of N,N-dimethylisopropanolamine was 98.1%, and the crude product was synthesized with a color of 8APHA.

[0044] 2. Carry out continuous rectification of the crude product, the vacuum degree is -0.099MPa, the feed temperature is 100°C, the tower top cut-off temperature is 53°C, the purity of the refined N,N-dimethylisopropanolamine product is ≥99.5%, and the color The chromaticity is 0 APHA, the chromaticity is 10 APHA after 90 days at room temperature, and the chromaticity is 70 APHA after 7 days at 60°C.

[0045] 3. After th...

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Abstract

The invention discloses a preparation method for alkyl alcohol amine. The preparation method comprises the following steps: (1) feeding alkyl amine and a reaction promoter alkanolamine into a reaction kettle for stirring and mixing; (2) adding epoxy alkane for synthesis, wherein the feeding molar ratio of epoxy alkane for synthesis to alkyl amine is higher than the theoretical reaction molar ratio; (3) after the feeding is finished, carrying out heating and pressurization; (4) carrying out heat preservation conversion rate to obtain a crude product; (5) conducting continuous distillation on the crude product to separate out alkyl alcohol amine. During the preparation, alkanolamine is primary alkanolamine or secondary alkanolamine. Compared with the prior art, the preparation method provided by the invention adopts the technical scheme that alkanolamine is taken as the reaction promoter instead of water as a catalyst, so that the conversion rate of alkyl amine can reach 99.0% in general, the highest conversion rate can reach 99.9%, and the highest recovery rate of alkyl alcohol amine can reach 99.8%. Therefore, the preparation method provided by the invention has the advantages of being high in raw material conversion rate and recovery rate.

Description

technical field [0001] The invention relates to a preparation method of alkanolamine. Background technique [0002] Most of the existing alkanolamine production technologies adopt batch reaction or continuous production. The common feature of these processes is that most of them use water as a synthesis reaction catalyst, and in order to suppress the formation of polyether by-products, an excessive amount of Alkylamine, adopt 2.5~50% water as catalyzer in the patent CN103261130A, the feed molar ratio of ethylene oxide and dialkylamine is 1: 1.1~10, because the oxyethane and dialkylamine Reaction molar ratio is 1: 1, and in this document, the consumption of alkylamine is excessive, and the feed molar ratio of alkylene oxide and alkylamine is 0.10~0.91 times of its theoretical reaction molar ratio, and as in the patent US2337004A It is also mentioned that excessive alkylamines can significantly inhibit the generation of by-products, but due to the excess of amines, after the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/08C07C215/12C07C213/10C07C213/04
Inventor 汪少平张书田秀娟杭建荣
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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