Preparation method of tertiary amine-terminated polyether nonionic surfactant
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A technology of terminal tertiary amino group polyether and non-ionic surface, which is applied in the field of preparation of tertiary amino group terminal polyether type nonionic surfactant, can solve the problems of long reaction time and cumbersome process, and achieves short reaction time and reaction time. The effect of high activity and large production capacity
Active Publication Date: 2022-08-09
JIANGNAN UNIV
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[0007] Method 4: Chinese patent CN113061242A discloses a polyetheramine compound, its preparation method and application, specifically, it is terminated by a tertiary amino group with one active group The compound is used as an initiator, and the alkoxylation reaction is carried out to synthesize a preliminary polyether, and the preliminary polyether is subjected to a transesterification reaction to obtain a terminally modified polyether compound; this reaction needs to be carried out step by step, the process is cumbersome, and the reaction time is relatively long long
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Embodiment 1
[0035] Preparation of supported catalysts
[0036] (1) Place 60 g of commercially available carbon nanotubes in 300 mL of mixed acid solution (HNO 3 :H 2 SO 4 =3:1), ultrasonically treated for 2 hours at room temperature to obtain modified carbon nanotubes rich in a large number of oxygen-containing functional groups, diluted with 800 mL of deionized water, and then vacuum filtered. The solid obtained by suction filtration was washed with a large amount of deionized water until the pH of the deionized water after washing was neutral, and then the solid was vacuum-dried at 70 °C for 2 h to obtain the carrier f-MWCNTs.
[0037] (2) The carrier f-MWCNTs obtained in step (1) was placed in 500 mL of deionized water, and ultrasonically stirred at room temperature for 2 h, and then 145.4 g of Ni(NO 3 ) 2 , 55.8g of Cu (NO 3 ) 2 , 19.9g of H 8 N 2 O 4 The metal salt of W was dispersed in the above solution, and ultrasonic stirring was continued for 2h. After stirring, the mi...
Embodiment 2
[0040] The only difference from Example 1 is that the vacuum-dried solid matter in step (2) is calcined in a muffle furnace at 320° C. for 5 hours, and the remaining steps are the same as those in Example 1.
[0041] In the finally obtained supported catalyst Ni-Cu-W / f-MWCNTs, Ni, Cu, and W account for 4.5%, 2.5%, and 2.0% of the total weight of the supported catalyst, respectively.
Embodiment 3
[0043] The only difference from Example 1 is that the vacuum-dried solid matter in step (2) is calcined in a muffle furnace at 320° C. for 10 hours, and the remaining steps are the same as those in Example 1.
[0044] In the finally obtained supported catalyst Ni-Cu-W / f-MWCNTs, Ni, Cu, and W account for 4.7%, 3.0%, and 2.2% of the total weight of the supported catalyst, respectively.
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Abstract
The invention discloses a preparation method of a tertiary amine-terminated polyether nonionic surfactant, and belongs to the field of chemical synthesis technologies and surfactants. The preparation method comprises the following steps: (1) placing a supported catalyst in a fixed bed, and preheating the fixed bed; dissolving polyether amine and paraformaldehyde in a solvent to obtain a dissolved solution; then injecting the dissolved solution into a fixed bed, replacing air in the fixed bed with hydrogen, pressurizing the fixed bed with hydrogen, and carrying out a reaction; (2) after the reaction is finished, collecting feed liquid; and after the feed liquid is cooled, filtering and carrying out reduced pressure distillation to obtain the tertiary amine-terminated polyether. The method for continuously producing the tertiary amine-terminated polyether by using the fixed bed has the characteristics of safety, convenience in operation, short reaction time, few side reactions and suitability for large-scale production; the conversion rate of the primary amine is high, the selectivity of the tertiary amine is good, the yield of the tertiary amine-terminated polyether is up to 98.2%, and meanwhile, the tertiary amine-terminated polyether also has better surface activity.
Description
technical field [0001] The invention relates to a preparation method of a terminal tertiary amine group polyether type nonionic surfactant, belonging to the fields of chemical synthesis technology and surfactants. Background technique [0002] Amine-terminated polyether is a kind of polyoxyolefin compound terminated by amine group. Its special structure makes it widely used in polyurethane (urea), polyurea material, epoxy resin curing agent, anti-corrosion coating, jewelry manufacturing and surface active agents, etc. According to the difference in molecular weight and the number of functional groups, amino-terminated polyethers can be divided into various series of products. Conventional amino-terminated polyether products are generally primary amino-terminated polyether, secondary amino-terminated polyether and tertiary amino-terminated polyether. Tertiary amino-terminated polyethers have the characteristics of increasing the hydrophilicity, adsorption and antistatic prop...
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