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Method for separating C-type lignin and G/S-type lignin from Euphorbiaceae plant seed coats

A technology of lignin and Euphorbiaceae, applied in the field of lignin, can solve the problems of unclear structure purity, many steps, low purity, etc., and achieve the effect of efficient complete separation, high C-type lignin content, and excellent yield

Active Publication Date: 2021-09-21
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the previous literature, the team of Professor Anastas of Yale University used methanol, dichloromethane and ethyl acetate to continuously extract the seed coat of the chestnut, but the sample did not undergo structural characterization, and there were many steps (three steps), and the yield Problems with low and unclear structural purity
The inventor's team has also reported the method of using deep eutectic solvents (DESs) to extract C-type lignin from castor seed coats. The C-type lignin sample yield reaches 17wt% (170g / kg seed coat), and the real The unit purity of cafestol (that is, C-type lignin content) is 31%, which is relatively low, and the deep eutectic solvent needs to be removed later, resulting in higher costs
Up to now, there is no report that can realize the high-efficiency separation of C-type lignin and G / S-type lignin on an industrial scale.

Method used

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  • Method for separating C-type lignin and G/S-type lignin from Euphorbiaceae plant seed coats
  • Method for separating C-type lignin and G/S-type lignin from Euphorbiaceae plant seed coats
  • Method for separating C-type lignin and G/S-type lignin from Euphorbiaceae plant seed coats

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 Comparison of various methods for preparing lignin

[0040] Sulfuric acid type C lignin (KL): Jatropha curcas seed coat powder (60 mesh, 2 g) was dissolved in 12 M sulfuric acid (20 mL) at 30 o C for 1 h, and then deionized water (560 mL) was added. at 120 o After further heating at C for 1 h, the mixture was filtered through a filter crucible (filter diameter 4–7 μm). Klason lignin (900 mg) was obtained as a solid.

[0041] Enzymatic Lignin (EL): Ball-milled Jatropha curcas seed coat (300 mesh, 10 g) was treated with cellulase (200000 μ / g, 750 mg) and xylanase (290000 μ / g, 750 mg) in citric acid Salt buffer (200 ml, pH = 4.8) at 50 o C in a shaker for 48 h. After enzymatic digestion, the solid residue was collected by centrifugation and treated again with cellulase and xylanase. The insoluble solid was collected, washed with deionized water, and lyophilized to give EL (7.8 g).

[0042] Enzymatic mild acid hydrolysis of lignin (EMAL): Enzymatic hydrol...

Embodiment 2

[0065] Extraction of Jatropha curcas seed coat by dioxane in the absence of hydrochloric acid at 85 o The yield of the lignin sample obtained for 3 h at C was 40 mg / g, and the measured C / (G+S) value was 10.5, which was close to the value obtained from 18 mM HCl solution (10.3). The production of C-type lignin and G / S lignin increased with acidity, while the relative content of C-type units decreased. For example, in the case of 360 mM HCl, the value of C / (G+S) dropped to 1.5, indicating that the acidic condition is not conducive to the separation of type C lignin. Under different hydrochloric acid concentrations, lignin yield and C-type lignin content are shown in Table 2 below:

[0066] Table 2

[0067]

[0068] In 18 mM HCl dioxane solution, temperature range from 55 to 95 o C was also studied, and the results are shown in Table 3 below:

[0069] table 3

[0070]

[0071] High temperature can significantly increase the yield of isolated lignin samples. at 55 o C...

Embodiment 3

[0073] To investigate the effect of compound solvents on the separation, concentrated HCl was added to the seed coat powder (60 mesh, 10 g). In the suspension formed by 100 mL of mixed solutions of dioxane and ethanol in different proportions, the concentration of [HCl] was about 18 mmol L -1 . Put the mixture in N 2 under 95 o C was heated for 3 h, and the solid residue was removed by centrifugation. The supernatant was concentrated by evaporation to obtain a concentrate, which was added to an aqueous hydrochloric acid solution at pH = 2.0. The formed precipitate was collected by centrifugation and freeze-drying to obtain the lignin product MIX. The results are listed in Table 4 below, and the solvent ratios are volume ratios (v / v):

[0074] Table 4

[0075]

[0076] According to the data in Table 4, the mixed solvent of dioxane and ethanol according to the volume ratio of 1-3:1-3 has the best separation effect of C-type lignin, and the lignin yield and C-type lignin...

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Abstract

The invention relates to a method for separating C-type lignin and G / S-type lignin from Euphorbiaceae plant seed coats, and the method comprises the following steps: crushing the Euphorbiaceae plant seed coats, performing heating, centrifuging and concentrating in an inert atmosphere by using an alcohol solvent and / or an oxygen heterocyclic ring solvent under a dilute acid condition to obtain a concentrated solution, adding the concentrated solution into an acidic aqueous solution, performing centrifuging and drying, and finally obtaining the lignin with high C-type content. According to the method, the C-type lignin and the G / S-type lignin are simply and efficiently separated from the Euphorbiaceae seed coats (jatropha curcas, swallow chestnut, tung oil tree and castor-oil plant) which are relatively cheap and wide in source, and the method has excellent yield and higher C-type lignin content. The separated C-type lignin biopolymer provides a single catechol derivative product through palladium-carbon catalytic hydrogenolysis, and possibility is provided for producing catechol compounds from green carbon raw materials.

Description

technical field [0001] The invention belongs to the field of lignin, and in particular relates to a method for separating C-type lignin and G / S-type lignin from Euphorbiaceae seed coats. Background technique [0002] Using biomass as hydrocarbon raw material to produce chemicals, energy and materials is one of the important ways to solve the shortage of fossil resources and achieve carbon peak and carbon balance. As the main component of biomass (20-30%), lignin is the largest renewable aromatic hydrocarbon resource in nature. Degrading lignin to aromatic compounds suitable for downstream processing and utilization can reduce dependence on petrochemical resources. In woody, herbaceous plants and most seed coats, lignin is composed of three kinds of monolignyl alcohols p-coumaryl alcohol (H), coniferyl alcohol (G) and sinapyl alcohol (S) to form biomacromolecules through oxidative polymerization, among which Ether chemical bonds such as β-O-4, β-β and β-5 are the main linkag...

Claims

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Application Information

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IPC IPC(8): C08H7/00C07C37/52C07C39/11
CPCC08H6/00C07C37/52
Inventor 宋国勇苏世浩王水众李赫龙沈清如
Owner BEIJING FORESTRY UNIVERSITY
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