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Method for preparing tri-isopropanolamine

A technology of triisopropanolamine and isopropanolamine, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve difficulties in the purity, water content and chroma of triisopropanolamine products Meet the quality requirements and other issues to achieve the effect of meeting market needs, saving costs and reducing energy consumption

Active Publication Date: 2008-09-17
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is that the purity, water content, chroma and other indicators of the triisopropanolamine product produced by the existing method are difficult to meet the quality requirements for the preparation of high-end products such as medicine and new polymer materials, Provide a kind of synthetic method of new triisopropanolamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Existing one 10M 3 For the reaction kettle, first vacuum the reaction kettle to -0.0985MPa, and then inject high-purity nitrogen to a pressure of 0.30MPa to vacuum, and replace it three times in this way. Under the protection of nitrogen, 5000Kg of isopropanolamine (30% of monoisopropanolamine, 69.9% of diisopropanolamine, and 0.1% moisture) and 3870Kg of propylene oxide were pumped into the reactor. , Start stirring, control the reaction temperature at 80-85°C, control the reaction pressure at -0.08~0.50Mpa, continue stirring for 8 hours, and take samples for testing. Test results: 99.3% triisopropanolamine, 0.1% moisture content, and 0.6% diisopropanolamine. After storing the product at room temperature for 180 days, the detected moisture content is 0.15%, the appearance is white crystalline solid, and it melts into liquid Pt-Co with color code within 30.

Embodiment 2

[0016] Existing one 10M 3 For the reaction kettle, first vacuum the reaction kettle to -0.0982MPa, and then inject high-purity nitrogen to a pressure of 0.28MPa to vacuum, and replace it for 5 times. Under the protection of nitrogen, 5000Kg of monoisopropanolamine (containing monoisopropanolamine isomers) with a purity of 99.9% and a water content of 0.1% and 8112Kg of propylene oxide were pumped into the reactor respectively. , Start stirring, control the reaction temperature at 80-85°C, control the reaction pressure at 0~0.70Mpa, continue stirring for 8 hours, and take samples for testing. Test results: 99.2% triisopropanolamine, 0.1% moisture content, and 0.7% diisopropanolamine. After storing the product at room temperature for 180 days, the detected moisture content is 0.15%, the appearance is a white crystalline solid, and it melts into a liquid Pt-Co with a color number of less than 20.

Embodiment 3

[0018] Existing one 10M 3 For the reaction kettle, first vacuum the reaction kettle to -0.0989MPa, and then inject high-purity nitrogen to a pressure of 0.35MPa to vacuum, and replace it 4 times in this way. Under the protection of high-purity nitrogen, 5000Kg of diisopropanolamine (containing diisopropanolamine isomers) with a purity of 99.9% and a water content of 0.1% and 2256Kg of propylene oxide were pumped to the reaction. In the kettle, start stirring, control the reaction temperature at 80-85°C, and control the reaction pressure at -0.03~0.70Mpa, continue stirring for 8 hours, and take samples for testing. Test results: 99.4% triisopropanolamine, 0.1% moisture, 0.5% diisopropanolamine. After storing the product at room temperature for 180 days, the detected moisture content is 0.15%, the appearance is a white crystalline solid, and it melts into liquid Pt-Co with a color code of less than 15.

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Abstract

The invention relates to a method of manufacturing triisopropanolamine. Firstly, air in a reaction kettle is replaced by nitrogen, and the reaction kettle is vacuumized; then after being injected with the nitrogen, the reaction kettle is vacuumized; the step is repeated for three to five times; secondly, isopropanolamine or diisopropanolamine or isopropanolamine mixture are put in the reaction kettle, the nitrogen is injected until the pressure reach more than minus 0.05MPa, then propylene oxide is added in continuously, wherein, the molar ratio between the propylene oxide and the number of hydrogen atoms contained on nitrogen atoms in the isopropanolamine is controlled within 1.0 to 1.1, the reaction temperature ranges from 50 to 90 DEG C, the reaction pressure ranges from minus 0.1 to 1.0MPa, and the reaction time is 8 to 15 hours; after the reaction is finished, products are discharged and packed under the protection of the nitrogen. The method greatly lowers the energy consumption, reduces the caused environmental pollution, increases the product quality, has low demand to equipment, saves the cost, has wide demanding range to raw material, and can make the best of waste materials which are generated when manufacturing the isopropanolamine and the diisopropanolamine. The purity of the products which is manufactured by adopting the method can reach more than 99 percent, the moisture content is less than 0.3 percent, and the colority of Pt-Co is less than 50.

Description

Technical field [0001] The invention relates to a method for preparing triisopropanolamine. Background technique [0002] Triisopropanolamine is a white or slightly yellow solid at room temperature, its scientific name is 1,1’,1”-nitrilotripropan-2-ol, and its chemical formula is (CH 3 CHOHCH 2 ) 3 N. Triisopropanolamine has a wide range of uses. It can be used as an auxiliary filler in the rubber industry; it can be used as a chain terminator for certain polymerization reactions; it can be used as a raw material for various cosmetic creams, woolen fabrics and wool detergents; It is used in fiber oil, cutting oil and latex paint; it can be used in the synthesis of drugs and new polymer materials. The zincate zinc plating additive made from triisopropanolamine can also be used in non-cyanide electroplating process to make the electroplating layer smooth, bright, strong adhesion and corrosion resistance. [0003] At present, in the industry, ammonia or liquid ammonia and propylene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/12C07C213/04
Inventor 张书杭建荣邢益斌
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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