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Catalyst for synthesis of amino-terminated polyether

A technology of amino-terminated polyether and catalyst, which is applied in the field of catalysis, can solve the problems of low reaction conversion rate and high reaction pressure of synthesizing amino-terminated polyether, and achieve good catalytic effect, reduced reaction cost and high primary amine selectivity.

Active Publication Date: 2015-04-22
HONGBAOLI GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Purpose of the invention: the purpose of the present invention is to solve the problems of high reaction pressure and low reaction conversion rate in the synthesis of amino-terminated polyether in the prior art, and to provide a high conversion rate and high-selectivity synthesis of amino-terminated polyether, and the reaction Catalyst for hydroamination reaction with mild conditions and preparation method thereof

Method used

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  • Catalyst for synthesis of amino-terminated polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take by weighing 56.7g nickel nitrate Ni (NO 3 ) 2 , 6.3g cobalt nitrate Co(NO 3 ) 2 , 0.34g chromium nitrate Cr(NO 3 ) 2 , 0.3g molybdenum nitrate Mo(NO 3 ) 2 (The mass ratio of Ni and Co is about 90:10, and the mass ratio of the main active material Ni, Co and auxiliary active material Cr and Mo is about 99:1) and 5g of carrier Al 2 o 3 (carrier and catalyst mass ratio about 20:80) is placed in 35ml deionized water, the mass concentration of metal salt solution is about 65%; Heating and stirring metal salt solution to 60 ℃, after 10min, add dropwise to it the mass fraction of 30% NaCO 3 The solution was 90ml, the dropping rate was 5ml / min, and after the addition was completed, it was aged at 60°C for 1h; after the aging was completed, it was suction-filtered, washed twice with deionized water and absolute ethanol, and then vacuum-dried at 100°C for 2h. Calcined at 500°C for 2 hours; after the calcination, the obtained catalyst was ground to 60 mesh and sieved...

Embodiment 2

[0024] Weigh 56.7g nickel nitrate Ni (NO 3 ) 2 , 6.3g cobalt nitrate Co(NO 3 ) 2 , 1.0g chromium nitrate Cr(NO 3 ) 2 , 2.3g molybdenum nitrate Mo(NO 3 ) 2 (The mass ratio of Ni and Co is about 90:10, and the mass ratio of the main active material Ni, Co and auxiliary active material Cr and Mo is about 95:5) and 5.4g of carrier Al 2 o 3 (The mass ratio of the carrier to the catalyst is about 20:80) placed in 33ml deionized water, the mass concentration of the metal salt solution is about 68%; heat and stir the metal salt solution to 70°C, and after 10min, dropwise add NaCO with a mass fraction of 35% 3 The solution was 85ml, the dropping rate was 4ml / min, and after the addition was completed, it was aged at 70°C for 1h; after the aging was completed, it was suction filtered, and washed twice with deionized water and absolute ethanol, and then vacuum-dried at 100°C for 2h, and then Calcined at 450°C for 2.5h; after the calcination, the obtained catalyst was ground to 60 ...

Embodiment 3

[0026] Weigh 56.4g nickel acetate Ni(CH 3 COO) 2 , 6.6g cobalt acetate Co(CH3 COO) 2 , 10.0g iron acetate Fe(CH 3 COO) 3 , 10.0g molybdenum acetate Mo(CH 3 COO) 2 (Ni, Co mass ratio 90:10, Ni, Co and Fe, Mo mass ratio 80:20), 6.9g carrier Al 2 o 3 and 4g of TiO 2 (Mass ratio of carrier to catalyst 25:75) was placed in 29.7ml deionized water, and a metal salt solution with a mass concentration of 70% was prepared; heated and stirred to 70°C, and after 20min, 40% NaCO was added dropwise 3 The solution is 80ml, the dropping rate is 3ml / min, after the end, it is aged at 80°C for 1h; it is suction filtered and washed 3 times with deionized water and absolute ethanol respectively, and then vacuum-dried at 100°C for 3h, and then calcined at 400°C for 4h ; After the calcination ends, the catalyst is ground to 30 mesh and sieved, and then with 20% H 2 / 80%N 2 The mixed gas was reduced at 160° C. for 1.5 h to obtain 35 g of black solid powder catalyst. The catalyst was sealed...

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Abstract

The invention discloses a catalyst for synthesis of amino-terminated polyether. The catalyst is load type, the carrier material has a porous structure, metal Ni and Co are taken as the main active components of the catalytic material, and any two of Cr, Fe and Mo are mixed in any proportion to serve as the assistant active component. The invention discloses a preparation method of the catalyst and application of the catalyst to synthesis of amino-terminated polyether. The catalyst provided by the invention is used for synthesis of amino-terminated polyether, and also has high conversion rate and high primary amine selectivity that are both greater than or equal to 99.0%. By using the catalyst provided by the invention, the reaction cost is lowered, and the catalyst has good catalytic effect in a batch kettle and a fixed bed reactor, and can meet different process requirements. By adding the catalyst, the reaction can be milder and more controllable, the temperature is lower than or equal to 230DEG C, the pressure is less than or equal to 10MPa, and the risk of the operation process is reduced.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a catalyst for synthesizing amino-terminated polyether and a preparation method thereof. Background technique [0002] Amine-Terminated Polyether (ATPE), also known as polyether amine, is a kind of polyoxyalkylene compound, the main chain of which is a polyether skeleton, but the end is blocked by an amino group. According to the number of substituted H atoms in the amino group, it can be divided into primary amino group and secondary amino group terminated amino polyether. At present, the international market of amino-terminated polyether products is mainly monopolized by Huntsman and Basf, and only a few companies in China can produce them, but the reaction conversion rate and product selectivity are quite different from those of foreign companies, and the product quality is unstable, and their production capacity is also low. Can not meet the needs of the domest...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/887B01J23/883C08G65/325
Inventor 邢益辉沈小勇唐黎余渡江
Owner HONGBAOLI GRP CO LTD
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