WO2020087201A1

WO2020087201A1 - Comprehensive preparation method for bamboo biological extracts and bamboo fibre

Info

Publication number: WO2020087201A1
Application number: PCT/CN2018/112395
Authority: WO
Inventors: 张毅; 陈燕梅
Original assignee: 张毅
Priority date: 2018-10-29
Filing date: 2018-10-29
Publication date: 2020-05-07

Abstract

A comprehensive preparation method for bamboo biological extracts and bamboo fibre, comprising: (1) preparing bamboo shavings; (2) extracting bamboo green extract and bamboo shavings polysaccharide mixed crude extract; (3) separating the bamboo green extract and the bamboo shavings polysaccharide mixed crude extract; and (4) preparing the bamboo green extract. Biological extracts such as bamboo green extract, bamboo polysaccharides, and bamboo sap solution can be extracted from bamboo, and the residual bamboo material obtained after extraction, such as bamboo shavings and bamboo flesh (including Shiraia bambusicola) can synchronously prepare bamboo fibre, effectively enhancing the rate of utilisation of the bamboo and the added value; the extraction steps are simple, no de-waxing step is required, and the amount of organic solvent used is significantly reduced; the difficulty of biological degumming of bamboo fibre is effectively reduced, increasing the strength of the bamboo fibre; efficient and comprehensive utilisation of bamboo resources is achieved, and the conditions for the green production of bamboo fibre are created.

Description

Comprehensive preparation method of bamboo biological extract and bamboo fiber

【Technical Field】

The invention specifically relates to a comprehensive preparation method of bamboo biological extract and bamboo fiber.

【Background technique】

Bamboo is the main part of the bamboo and leaves after the felling of the bamboo, also known as bamboo stalks. Its cross-section consists of three layers: bamboo green, bamboo meat, and bamboo yellow. The bamboo green is also composed of the outer skin, namely the gray matter layer and the superficial fiber layer, which is thrown away as waste by general bamboo processing (production of bamboo flooring, bamboo fiber, etc.). Astaxanthin can be extracted from the superficial fiber layer of bamboo materials, and is widely used as a food and feed additive, which can significantly improve the edible quality and nutritional value.

In terms of chemical composition, bamboo mainly includes cellulose, hemicellulose and lignin. Hemicellulose is mainly composed of five-carbon sugar and six-carbon sugar, including xylose, arabinose and galactose, also known as polysaccharides. The superficial fiber layer and the bamboo meat part contain a large amount of hemicellulose, or polysaccharide. The polysaccharide can be used as a broad-spectrum immune promoter, and has various biological effects such as antioxidant, anti-tumor, and hypoglycemic. The Chinese patent "Extraction method of bamboo polysaccharide" with the application number CN201310064648.0 and the Chinese patent "A kind of bamboo polysaccharide of Lingnan Mountain and its preparation method and application" with the application number CN201310536026.3 both use steam blasting method to refine bamboo materials This method has the disadvantages of high energy consumption, short bamboo fiber length, low strength, etc., which is not conducive to comprehensive utilization, and the extraction component is single.

[Invention content]

The technical problem to be solved by the present invention is to provide a comprehensive preparation method of bamboo biological extracts and bamboo fibers, to carry out comprehensive development of bamboo resources, so as to make the best use of materials and efficient use.

The invention is realized in this way: the comprehensive preparation method of bamboo biological extract and bamboo fiber includes the following steps:

(1) Preparation of bamboo ru: remove the bamboo branches and leaves, scrape the bamboo into silk or slice into thin slices to obtain bamboo ru, the remaining part is the bamboo residue;

(2a) Extraction of mixed crude extract: Use methanol or ethanol or a mixture of the two with a content of more than 75%, slowly add caustic soda, fully stir to dissolve to saturation, and configure to be alkaline methanol or ethanol. Zhuru is placed in alkaline methanol or alkaline ethanol solution or a mixture of the two, and is extracted 1-3 times by the coexistence of percolation method and reflux method, 1-3 hours each time, in which the mass ratio of the material to the liquid is 1 : 3-1: 10, pH greater than 8, temperature 40 ℃ -70 ℃; concentrate the extract to obtain the mixed crude extract of bamboo green polysaccharide and bamboo polysaccharide;

(3) Separation: add 3-5 times (w / v) water to the mixed crude extract, adjust the pH to 3-5, stir until the extract forms flocs, filter out the liquid, and then use the same Method Wash the flocs twice, and then combine the three washing liquids;

(4) Preparation of bamboo green pigment: the flocs are subjected to one or several solvents in 1-5 times (w / v) of petroleum ether, 6 # extraction solvent oil, n-hexane and ethyl acetate. Extract 1-3 times, combine the extracts, and concentrate to obtain cinnabarin.

Preferably, it also includes:

(5) Preparation of Polysaccharides from Bamboo Ru: concentrate the washing solution obtained in (3) to a specific gravity of 1.1-1.3, naturally cool to room temperature, add caustic soda to neutralize to neutrality, add 3-5 times the amount (w / v) Ethanol, stir, let stand at 0-10 ° C for 12h, collect the precipitate, and wash with 80% ethanol to get the bamboo polysaccharide.

Preferably, it also includes:

(2b) Preparation of bamboo leach: After opening the bamboo residue obtained in (1), add 5-10 times the amount (w / v) of purified water, decoction at 100 ℃ for 2-3h, repeat 1-3 times , Combine the decoction, filter, and concentrate the filtrate to a specific gravity of concentrated juice of 1.05-1.2 to obtain bamboo leachate.

Preferably, it also includes:

(6) Preparation of bamboo fiber: combine the bamboo residue after extraction with (2a) and the bamboo residue after extraction with (2b), and deliver to the continuous degumming tank equipped with biological compound enzyme solution for degumming, 30 ℃ -60 Insulate at ℃ for 1-2h, then drain, dry and comb to obtain natural bamboo fiber. .

Preferably, the biological composite enzyme solution includes: 20g / L-50g / L laccase and 20g / L-50g / L xylanase.

Preferably, in said (3), dilute hydrochloric acid, dilute sulfuric acid and dilute nitric acid are used to adjust the pH value.

The advantage of the invention is that not only can biological extracts such as astaxanthin, bamboo polysaccharides, bamboo leach, etc. be extracted from bamboo, but also bamboo residues and bamboo meat (including bamboo yellow) and other bamboo residues obtained after extraction can be prepared simultaneously Bamboo fiber effectively improves the utilization rate and added value of bamboo materials; the extraction step is simple, no need to go through the wax removal step, the amount of organic solvent is significantly reduced; the difficulty of biological degumming of bamboo fiber is effectively reduced, which is conducive to improving the strength of bamboo fiber; The efficient and comprehensive utilization of bamboo resources also creates conditions for the green production of bamboo fibers.

【Explanation】

The present invention will be further described below with reference to the drawings and embodiments.

FIG. 1 is a process flow diagram of the comprehensive preparation method of bamboo biological extract and bamboo fiber of the present invention.

【detailed description】

Example 1

As shown in Figure 1, the comprehensive preparation method of bamboo biological extract and bamboo fiber includes the following steps:

(1) Preparation of bamboo ruthenium: remove bamboo branches and leaves, scrape bamboo material into silk strips or cut into thin slices to obtain bamboo ruthenium, the remaining part is bamboo meat (including bamboo yellow);

(2a) Extraction of mixed crude extract: Use methanol or ethanol with a content of more than 75%, slowly add caustic soda, fully stir to dissolve to saturation, and configure as alkaline methanol. Zhuru is placed in alkaline methanol solution and extracted by coexistence of percolation method and reflux method for 1 hour each time. Among them, the material-to-liquid mass ratio is 1: 3, the pH is greater than 8, and the temperature is 40 ° C; concentration The extract is obtained by mixing crude extracts of bamboo green pigment and bamboo polysaccharide;

(2b) Preparation of bamboo leach: after opening the bamboo meat (including bamboo yellow) obtained in (1), add 5 times the amount (w / v) of purified water, cook at 100 ° C for 2h, repeat 1 time, combine The decoction is filtered, and the filtrate is concentrated until the specific gravity of the concentrated juice is 1.05 to obtain bamboo leach.

(3) Separation: add 3 times the amount of (w / v) water to the mixed crude extract, adjust the pH to 3 with dilute sulfuric acid, stir until the extract forms flocs, filter out the liquid, and then use the same method Wash the flocs twice, and then combine the three washing liquids;

(4) Preparation of bamboo green pigment: the floc is extracted twice with 1 times the amount (w / v) of petroleum ether, the extracts are combined and concentrated to obtain bamboo green pigment.

(5) Preparation of bamboo Ru polysaccharide: concentrate the washing liquid obtained in (3) to a specific gravity of 1.1, naturally cool to room temperature, add caustic soda to neutralize to neutrality, add 3 times the amount (w / v) of ethanol, and stir ， Stand at 0 ℃ for 12h, collect the precipitate, and wash with 80% ethanol to obtain the bamboo polysaccharide.

(6) Preparation of bamboo fiber: combine the bamboo residues extracted by (2a) and the bamboo residues extracted by (2b), and transport them to a continuous degumming tank equipped with biological compound enzyme solution for degumming, and keep at 60 ℃ for 1h , Then drain, dry and comb to get natural bamboo fiber. The biological compound enzyme solution includes: 20 g / L of laccase and 20 g / L of xylanase.

Example 2

(2a) Extraction of mixed crude extract: use ethanol with a content of more than 75%, slowly add caustic soda, fully stir to dissolve to saturation, and configure it as alkaline ethanol. Zhuru is placed in alkaline ethanol solution and extracted three times by coexistence of percolation method and reflux method, each time for 3 hours. Among them, the mass ratio of material to liquid is 1:10, pH is 10, temperature is 70 ℃; concentrated extraction Liquid, get the mixed crude extract of bamboo green pigment and bamboo polysaccharide;

(2b) Preparation of bamboo leaching solution: After opening the bamboo meat (including bamboo yellow) obtained in (1), add 10 times the amount (w / v) of purified water, cook at 100 ° C for 3h, repeat 3 times, combine The decoction is filtered, and the filtrate is concentrated to a specific gravity of 1.2 for concentrated juice to obtain bamboo leach.

(3) Separation: Add 5 times the amount of (w / v) water to the mixed crude extract, adjust the pH to 5 with dilute nitric acid, stir until the extract forms flocs, filter out the liquid, and then use the same method Wash the flocs twice, and then combine the three washing liquids;

(4) Preparation of bamboo green pigment: the flocs are extracted twice with 5 times the amount (w / v) of ethyl acetate three times, and the extracts are combined and concentrated to obtain bamboo green pigment.

(5) Preparation of Polysaccharides from Bamboo Ru: concentrate the washing liquid obtained in (3) to a specific gravity of 1.3, naturally cool to room temperature, add caustic soda to neutralize to neutrality, add 5 times the amount (w / v) of ethanol, and stir , Stand still at 10 ℃ for 12h, collect the precipitate, and wash with 80% ethanol to get the bamboo polysaccharide.

(6) Preparation of bamboo fiber: combine the bamboo residue after extraction with (2a) and the bamboo residue after extraction with (2b), transfer to the continuous degumming tank equipped with biological compound enzyme solution for degumming, and keep at 30 ℃ for 2h , Then drain, dry and comb to get natural bamboo fiber. The biological compound enzyme solution includes: 50 g / L of laccase and 50 g / L of xylanase.

Example 3

(2a) Extraction of mixed crude extract: Use a mixture of methanol and ethanol with a content of more than 75%, slowly add caustic soda, fully stir to dissolve to saturation, and configure an alkaline mixture of methanol and ethanol. Zhuru is placed in a mixed solution of alkaline methanol and ethanol, and extracted twice by coexistence of percolation method and reflux method, each time for 2 hours. Among them, the mass ratio of feed liquid is 1: 6, pH is greater than 8, temperature is 60 ℃; Concentrate the extracts to get the mixed crude extract of bamboo green pigment and bamboo polysaccharide;

(2b) Preparation of bamboo leaching solution: After the bamboo meat (including bamboo yellow) obtained in (1) is sliced, add 8 times the amount (w / v) of purified water, decoction at 100 ℃ for 2.5h, repeat 2 times, Combine the decoction, filter, and concentrate the filtrate to a specific gravity of 1.1 for concentrated juice to obtain bamboo leach.

(3) Separation: add 4 times (w / v) water to the mixed crude extract, and then adjust the pH to 4 with dilute hydrochloric acid, dilute sulfuric acid, and dilute nitric acid, stir until the extract forms flocs, and filter out Liquid, then wash the flocs twice in the same way, and then combine the three washing liquids;

(4) Preparation of bamboo green pigment: the flocs are extracted twice with 3 times (w / v) 6 # extraction solvent oil and n-hexane mixed liquid, and the extracts are combined and concentrated to obtain bamboo green pigment .

(5) Preparation of Zhuru polysaccharide: concentrate the washing liquid obtained in (3) to a specific gravity of 1.2, naturally cool to room temperature, add caustic soda to neutralize to neutrality, add 4 times the amount (w / v) of ethanol, and stir , Stand at 5 ℃ for 12h, collect the precipitate, and wash with 80% ethanol to obtain the bamboo polysaccharide.

(6) Preparation of bamboo fiber: combine the bamboo residues extracted by (2a) and the bamboo residues extracted by (2b), and transport them to a continuous degumming tank equipped with biological compound enzyme solution for degumming, and keep at 40 ℃ for 2h , Then drain, dry and comb to get natural bamboo fiber. The biological compound enzyme solution includes: 40 g / L of laccase and 30 g / L of xylanase.

The invention has the following advantages:

1. The present invention is directed to the efficient and comprehensive utilization of various components of bamboo materials, not only can extract biological extracts such as bamboo green pigments, bamboo polysaccharides, bamboo leach, etc. from bamboo materials, but also bamboo bamboo and bamboo meat (including bamboo yellow) after extraction ) The remaining bamboo materials can also be used to prepare bamboo fibers simultaneously, which effectively improves bamboo utilization and added value;

2. The present invention adopts a synchronous extraction method, which can simultaneously extract the abacin and bamboo polysaccharides from bamboo, the steps are simple, no wax removal step is needed, and the preparation of abacin in the separation process uses secondary extraction, and the amount of organic solvent Significantly reduced;

3. In the present invention, bamboo materials are first extracted from biological extracts and then prepared from bamboo fibers, which effectively reduces the difficulty of bamboo fiber biological degumming, helps to increase the strength of bamboo fibers, and creates conditions for green production of bamboo fibers.

Although the specific embodiments of the present invention have been described above, those skilled in the art should understand that the specific embodiments we have described are only illustrative, and are not intended to limit the scope of the present invention. Equivalent modifications and changes made by a technician in accordance with the spirit of the present invention should be covered by the scope of the claims of the present invention.

Claims

A comprehensive preparation method of bamboo biological extract and bamboo fiber is characterized by comprising the following steps:

(1) Preparation of bamboo ru: remove the bamboo branches and leaves, scrape the bamboo into silk or slice into thin slices to obtain bamboo ru, the remaining part is the bamboo residue;

(2a) Extract the mixed crude extract: use methanol or ethanol with a concentration of more than 75% or a mixture of the two, slowly add caustic soda, stir to dissolve to saturation, and obtain alkaline methanol or alkaline ethanol; In methanol or alkaline ethanol solution or a mixture of the two, extract 1-3 times by the coexistence of percolation method and reflux method, 1-3 hours each time, in which the mass ratio of feed liquid is 1: 3-1: 10 , PH is greater than 8, and the temperature is 40 ℃ -70 ℃; concentrate the extract to obtain the mixed crude extract of bamboo green pigment and bamboo polysaccharide;

(3) Separation: add 3-5 times (w / v) water to the mixed crude extract, adjust the pH to 3-5, stir until the extract forms flocs, filter out the liquid, and then use the same Method Wash the flocs twice, and then combine the three washing liquids;

(4) Preparation of bamboo green pigment: the flocs are subjected to one or several solvents in 1-5 times (w / v) of petroleum ether, 6 # extraction solvent oil, n-hexane and ethyl acetate. Extract 1-3 times, combine the extracts, and concentrate to obtain cinnabarin.
The comprehensive preparation method of bamboo biological extract and bamboo fiber according to claim 1, further comprising:

(5) Preparation of Polysaccharides from Bamboo Ru: concentrate the washing solution obtained in (3) to a specific gravity of 1.1-1.3, naturally cool to room temperature, add caustic soda to neutralize to neutrality, add 3-5 times the amount (w / v) Ethanol, stir, let stand at 0-10 ° C for 12h, collect the precipitate, and wash with 80% ethanol to get the bamboo polysaccharide.
The comprehensive preparation method of bamboo biological extract and bamboo fiber according to claim 1, further comprising:

(2b) Preparation of bamboo leach: After opening the bamboo residue obtained in (1), add 5-10 times the amount (w / v) of purified water, decoction at 100 ℃ for 2-3h, repeat 1-3 times , Combine the decoction, filter, and concentrate the filtrate to a specific gravity of concentrated juice of 1.05-1.2 to obtain bamboo leachate.
The method for comprehensive preparation of bamboo biological extract and bamboo fiber according to claim 3, further comprising:

(6) Preparation of bamboo fiber: combine the bamboo residue after extraction with (2a) and the bamboo residue after extraction with (2b), and deliver to the continuous degumming tank equipped with biological compound enzyme solution for degumming, 30 ℃ -60 Insulate at ℃ for 1-2h, then drain, dry and comb to obtain natural bamboo fiber. .
The comprehensive preparation method of bamboo biological extract and bamboo fiber according to claim 4, characterized in that the biological composite enzyme solution includes: 20g / L-50g / L laccase, 20g / L-50g / L Xylanase.
The method for comprehensively preparing a bamboo biological extract and bamboo fibers according to claim 1, wherein in (3), dilute hydrochloric acid, dilute sulfuric acid, and dilute nitric acid are used to adjust the pH value.