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Aminated lignin as well as preparation method and application thereof

A technology for aminating lignin and lignin, which is applied in the fields of building components, tar pitch/petroleum pitch/natural pitch processing, building insulation materials, etc. To avoid problems such as high degree of connection, achieve the effects of shortening the amination reaction time, high amination grafting rate, and increasing active sites

Pending Publication Date: 2020-06-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Purpose of the invention: The technical problem to be solved by the present invention is to solve the problems of slow reaction speed, high degree of crosslinking, low grafting ratio of amine groups, high energy consumption and low production efficiency in the synthesis process of lignin amination reaction in the prior art. , Difficult to achieve continuous production, complex post-processing, long time period and other problems, provide an aminated lignin and its preparation method

Method used

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  • Aminated lignin as well as preparation method and application thereof
  • Aminated lignin as well as preparation method and application thereof
  • Aminated lignin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: Degradation-acidolysis of lignin

[0039] In a 50mL reaction bottle, add 5g of lignin dissolved in 20mL of DMF, then add 5g of HBr with a mass fraction of 10%, and react in a microwave reactor at 90°C for 30min. After the reaction, the reactant was cooled to room temperature, added dropwise to 200 mL of 2% hydrochloric acid solution, stirred for 30 min, centrifuged, the precipitate was taken, washed with distilled water, washed until the supernatant was neutral, freeze-dried, Its NMR spectrum is as figure 1 Shown; the changes of molecular weight and hydroxyl before and after acid hydrolysis were detected by NMR and GPC [1] , the results are shown in the table below:

[0040] Table 1 Changes in molecular weight and phenolic hydroxyl groups of lignin before and after acidolysis

[0041]

Embodiment 2～5

[0042] Embodiment 2~5: the preparation of chlorohydrin intermediate

[0043] The aqueous solution of epichlorohydrin is configured in the first raw material storage tank, and the concentration of epichlorohydrin is 3mol / L, and the aqueous solution of aminating reagent diethylamine is configured in the second raw material storage tank, and the concentration is 3mol / L. Pump the first raw material storage tank (epichlorohydrin solution) and the second raw material storage tank (diethylamine aqueous solution) into the first micro-mixer in the microchannel reaction device according to the volume flow ratio of 1:1, mix and flow into The first microreactor, at a certain temperature, retain for a period of time, and take the reaction liquid GC-MS detection from the microstructure reactor I [2] Quantitative detection was carried out afterward, and the detection results are as follows:

[0044] Table 2 Epichlorohydrin and diethylamine reacted through microchannels and the intermediate ...

Embodiment 6～17

[0051] In the third raw material storage tank, configure acidolysis lignin alkali solution (prepared in embodiment 1), the proportioning of acidolysis lignin and (0.3mol / L) sodium hydroxide solution is 100g: 1L, the third raw material storage tank (acidolysis lignin alkaline solution) and the flow rate of the outlet of the first microreactor (embodiment 5), according to the volume flow ratio is 1:1 to pump in the microstructure reactor II, at a certain temperature, keep for a period of time, take The reaction liquid from the second micro-reactor is nano-filtered and spray-dried with a nano-filtration membrane with a molecular weight cut-off of 200-500 Da, and then elemental analysis and NMR are carried out. 1 H NMR ( image 3 ) for detection, the elemental analysis detection results are as follows:

[0052] Table 3 Nitrogen content of acid-hydrolyzed lignin through microchannel reaction and aminated lignin

[0053]

[0054]

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Abstract

The invention discloses aminated lignin as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) respectively pumping an epoxy chloropropane aqueous solution and an amination reagent aqueous solution into a first micro-mixer in a micro-channel reaction device at the same time, mixing, and introducing the mixture into a first micro-reactor in the micro-channel reaction device; and (2) while the step (1) is carried out, simultaneously pumping an alkali solution of the degraded lignin and the effluent of the first micro-reactor into a second mixer in the micro-reaction device, mixing, introducing the mixture into a second micro-reactor in the micro-reaction device, and collecting the effluent of the second micro-reactor, thereby obtaining the product. The method has the following advantages: (1) after pretreatment, the molecular weight is reduced, the phenolic hydroxyl group content is increased, and the reaction active sites are increased; and (2) the preparation process disclosed by the invention not only can realize continuous production, but also can shorten the amination reaction time, is low in energy consumption and improves the production efficiency.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to the application of aminated lignin and a preparation method thereof in asphalt emulsifiers. Background technique [0002] Coal, oil, natural gas and other fossil resources on the earth are non-renewable resources and are the main energy sources for human life and national industrial development. With the resource crisis and the increasing environmental awareness of human beings, the development of alternative resources is imminent. Lignin is a natural polymer with a complex structure. Its abundance in nature is second only to cellulose. It belongs to a class of effective renewable resources. resource. [0003] Asphalt is generally used in the form of hot asphalt, diluted asphalt, and emulsified asphalt. Emulsified asphalt refers to heating the viscous asphalt to a fluid state, and dispersing it in the form of extremely fine particles in an aqueous soluti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08J3/03C08L95/00C10C3/00
CPCC08H6/00C08J3/03C10C3/00C08J2395/00
Inventor 沈涛蔺熙珃朱晨杰应汉杰庄伟李明胡瑞佳黎明晖
Owner NANJING UNIV OF TECH
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