Method and device for preparing polyether amine

A technology of polyether amine and polyether polyol, which is applied in the field of organic chemical industry, can solve the problems of easy deactivation of catalysts, uneven loading, easy agglomeration, etc., and achieve large-scale continuous industrial production, excellent activity, and simple separation Effect

Active Publication Date: 2017-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large content of nickel loaded on the surface of the carrier during the preparation process, the catalyst is easily deactivated due to the disadvantages of easy agglomeration, sintering, and uneven loading during the preparation of the catalyst by the impregnation method, resulting in low reactivity.

Method used

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  • Method and device for preparing polyether amine
  • Method and device for preparing polyether amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Preparation and Application of 5%Ni-15%Re-1.2%B / SiO2 Catalyst

[0079] Weigh 10 grams of carrier SiO2 (20-40 mesh), put carrier SiO2 in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 10% ammonia-hydrogen gas mixture (molar content), ammoniation temperature The temperature is 300°C, and the ammoniation time is 5 hours. 2.477 g of Ni(NO3)2·6H2O, 2.161 g of NH4ReO4 and 0.686 g of H3BO3 were dissolved in 12 ml of deionized water. Half of this aqueous solution was used to impregnate the above-mentioned ammoniated SiO2 carrier, and then air-dried, then dried at 120° C. for 4 hours, and then calcined at 500° C. for 4 hours. Then, impregnate the ammoniated SiO2 carrier with the other half of the remaining aqueous solution for the second time, then dry it naturally, dry at 120° C. for 4 hours, and bake at 500° C. for 4 hours.

[0080] Weigh 3.2 grams (about 4 ml) of the above-mentioned catalyst and load it into a fixed-bed reactor. The catal...

Embodiment 2

[0082] Preparation and Application of 15%Ni-3.6%Re-1.2%B / SiO2 Catalyst

[0083] Weigh 10 grams of carrier SiO2 (20-40 mesh), put carrier SiO2 in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 20% ammonia-hydrogen gas mixture (molar content), ammoniation temperature The temperature is 300°C, and the ammoniation time is 5 hours. 7.432 grams of Ni(NO3)2·6H2O, 0.518 grams of NH4ReO4 and 0.686 grams of H3BO3 were dissolved in 12 ml of deionized water. Refer to Example 1 for the remaining preparation steps and catalyst evaluation scheme. The reaction conditions and reaction results are shown in Table 1.

Embodiment 3

[0085] Preparation and Application of 30%Ni-0.2%Re-15%K / SiO2 Catalyst

[0086]Weigh 10 grams of carrier SiO2 (20-40 mesh), put carrier SiO2 in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 50% ammonia-hydrogen gas mixture (molar content), ammoniation temperature The temperature is 300°C, and the ammoniation time is 5 hours. 14.864 grams of Ni(NO3)2·6H2O, 0.029 grams of NH4ReO4 and 3.879 grams of KNO3 were dissolved in 12 ml of deionized water. Refer to Example 1 for the remaining preparation steps and catalyst evaluation scheme. The reaction conditions and reaction results are shown in Table 1.

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Abstract

The invention relates to a method for preparing polyether amine by taking polyether polyol and ammonia as raw materials. The method comprises the following steps: mixing the polyether polyol and ammonia according to a certain ratio, pumping the mixture into a reactor by a pump, and reacting in the presence of a catalyst and hydrogen. A novel catalyst is adopted in the method and composed of three parts, namely a main active ingredient, aids and a carrier subjected to ammoniated treatment, wherein the main active ingredient refers to Ni or Co; the aids refer to one or more of metals such as Fe, Cu, Ru, Re, K, Zn and B or oxides; and the carrier subjected to ammoniated treatment is selected from SiO2 or Al2O3 subjected to ammoniated treatment. The catalyst in the invention has the characteristic that the adopted carrier needs to be subjected to special ammoniated treatment. According to the method disclosed by the invention, a reaction of performing polyether polyol and hydrogen present amination to produce polyether amine is carried out, and the method achieves high activity as well as high selectivity and stability.

Description

technical field [0001] The invention relates to a method and a device for preparing polyetheramine, which belong to the field of organic chemical industry. Background technique [0002] Polyether amine is a kind of amine compound containing special functional groups. Because it can react with a variety of groups, it is used in many fields in modern industry, such as: ion exchangers, lubricating oil additives, curing agents for epoxy resins , plasticizers and polyurethane (polyurea) materials, etc., and achieved good results. [0003] Experts and scholars at home and abroad have conducted in-depth and extensive research on the synthesis and application of polyetheramines. According to reports, foreign Huntsman companies have developed and industrialized production of lipopolyether amine products in the 1960s. The two internationally influential companies are Huntsman and BASF of the United States, which account for about 90% of the market share. In addition, Arch Company of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/325C08G65/48
Inventor 严丽丁云杰吕元
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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