A biomass fiber-based three-dimensional chromatography material and its preparation method

Abstract

The present invention discloses a biomass fiber-based three-dimensional chromatography material and a preparation method thereof. The preparation method of the chromatography material comprises the following steps: first extracting biomass fibers from natural plant stems and homogenizing and dispersing the biomass fibers to obtain biomass short fibers; then co-dispersing the biomass short fibers with natural high-molecular polysaccharides to prepare a biomass fiber composite slurry, and freeze-drying the composite slurry to obtain a biomass fiber three-dimensional precursor material; finally, modifying the precursor material to ultimately prepare a biomass fiber-based chromatography material with a stable three-dimensional structure. The three-dimensional chromatography material prepared by the present invention has both high protein adsorption capacity and processing throughput, and can achieve efficient protein separation and purification.

Description

Technical Field

[0001] The present invention relates to the field of functional textile materials, in particular to a biomass fiber-based three-dimensional chromatography material and a preparation method thereof. Background Art

[0002] Proteins have extremely broad and important applications in biomedicine, scientific research, food engineering and other fields. The purity and biological activity of proteins are key to ensuring their practical application performance. However, the protein content in the raw materials used in the production of protein products is usually low (less than 1%), so achieving efficient separation and purification of proteins is extremely critical. Among the many protein separation and purification methods, adsorption separation is widely used due to its advantages of easy operation, high processing efficiency and low cost. As the core of protein adsorption separation and purification technology, adsorption chromatography media directly determines the efficiency and cost of protein adsorption separation. Therefore, the development of high-efficiency protein adsorption separation chromatography media is of great significance to promoting the development of protein separation and purification technology.

[0003] Protein adsorption and separation chromatography media are usually functionalized porous resin gel microspheres or inorganic micron particle materials. The rich porous structure inside them gives them a high protein adsorption capacity, but they usually face disadvantages such as large mass transfer resistance, low separation and purification efficiency, and high energy consumption. Compared with traditional porous microsphere chromatography media, fibers have a larger aspect ratio, and their surface adsorption characteristics give them efficient and rapid protein adsorption and mass transfer capabilities. Constructing fibers into three-dimensional porous materials is expected to achieve better protein adsorption performance. At present, researchers have conducted some research on three-dimensional fiber materials for protein adsorption and separation, and have made certain research progress. However, the fiber raw materials used are mostly nanofibers prepared by electrospinning, hydrothermal synthesis and other technologies, which have problems such as complex preparation process, low production efficiency, and the use of organic solvents. Summary of the Invention

[0004] The purpose of the present invention is to provide a biomass fiber-based three-dimensional chromatography material and a preparation method thereof.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A biomass fiber-based three-dimensional chromatography material has a fiber framework porous structure composed of biomass fibers and a natural polymer polysaccharide binder, and is prepared by the following steps:

[0007] Step 1: extracting biomass fibers from natural plant stems and performing homogenization and dispersion treatment on the obtained biomass fibers to obtain biomass short fibers;

[0008] The natural plant stems are banana stems, lotus stems or taro stems;

[0009] Step 2: homogeneously co-dispersing the biomass short fibers obtained in step 1 with natural high molecular weight polysaccharides to obtain a biomass fiber composite slurry, and then freeze-drying the composite slurry to obtain a biomass fiber three-dimensional precursor material;

[0010] The natural high molecular weight polysaccharide is one or more of chitosan, gelatin, sodium alginate, and xanthan gum;

[0011] In the biomass fiber composite slurry, the concentration of biomass short fibers is 0.1-5%, and the concentration of natural high molecular weight polysaccharides is 0.05-2%.

[0012] Step 3, pre-immersing the precursor material obtained in step 2 in a modification solution, then freeze-drying the pre-immersed precursor material, heat-treating it after freeze-drying, and washing it with water until it is neutral, thereby obtaining a biomass fiber-based three-dimensional chromatography material;

[0013] The modified solution is a mixed solution of citric acid and a catalyst, the concentration of the citric acid is 0.1-20%, and the catalyst is concentrated sulfuric acid or polyphosphoric acid.

[0014] Furthermore, in step 1, the biomass fibers are extracted from the cross section of the natural plant stem using an extraction method.

[0015] Furthermore, the homogenous dispersion treatment in step 1 is to disperse the biomass fibers in deionized water and then disperse them by shearing. The speed of the shearing disperser is 1000-10000 rpm, and the dispersion time is 30-120 minutes.

[0016] Furthermore, the length of the biomass short fibers in step 1 is 10-200 μm.

[0017] Furthermore, the homogeneous dispersion conditions in step 2 are 1000-5000 rpm, and the dispersion time is 10-60 minutes.

[0018] Furthermore, the freeze-drying conditions in step 2 are a temperature of -20 to -80°C and a vacuum degree of 1 to 100 Pa.

[0019] Furthermore, the heat treatment in step 3 is performed at a temperature of 90-140° C. and for a time of 30-120 minutes.

[0020] The biomass fiber-based three-dimensional chromatography material of the present invention has a volume density of 2 to 100 mg / cm 3 The plastic deformation of cyclic compression in water is less than 10%, and the adsorption capacity for protein is 1000~3000mg / g.

[0021] The beneficial technical effects of the present invention are:

[0022] The present invention uses biomass fibers extracted from natural plant stems as raw materials, prepares biomass short fibers by shearing and dispersing the biomass fibers, and homogenizes and co-disperses the biomass short fibers with natural high-molecular polysaccharides, and combines freeze-drying and surface modification methods to prepare a three-dimensional chromatography material. The prepared biomass fiber-based three-dimensional chromatography material has a connected and regular fiber framework structure, and has good underwater compression mechanical properties and protein adsorption and separation properties. Its static protein adsorption capacity can reach 3000 mg / g. In addition, by filling the obtained biomass fiber-based three-dimensional chromatography material into an empty chromatography column, a commercial protein separation and purification chromatography column can be prepared.

[0023] The materials used in the preparation method provided by the present invention are all natural biomass raw materials, and the preparation process is simple, which is a green and environmentally friendly production method. Implementation Method

[0024] The preferred embodiments of the present invention will be described in detail below with reference to the examples. It should be understood that the following examples are provided for illustrative purposes only and are not intended to limit the scope of the present invention. Those skilled in the art may make various modifications and substitutions to the present invention without departing from the purpose and spirit of the present invention.

[0025] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0026] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources. Example 1

[0027] A biomass fiber-based three-dimensional chromatography material and a preparation method thereof, comprising the following steps:

[0028] (1) The long banana core fibers were extracted from natural banana stems. A small cutting machine was used to cut the long banana core fibers into short pieces. Then, deionized water was used as the solvent and the long banana core fibers were dispersed by a shearing disperser. During the dispersion process, the speed of the shearing disperser was 2000 rpm and the dispersion time was 30 minutes. The fiber dispersion was then dried to obtain short banana core fibers with an average fiber length of 150 μm.

[0029] (2) A certain amount of banana core fiber staple fibers and sodium alginate were homogenously dispersed in deionized water to prepare a fiber dispersion, wherein the concentration of biomass staple fibers was 0.5% and the concentration of sodium alginate was 0.1%. The speed of the homogenizer during the dispersion process was 1000 rpm and the dispersion time was 60 min. The prepared fiber dispersion was poured into a mold and then freeze-dried at a freezing temperature of -80 °C and a vacuum degree of 10 Pa to obtain a banana core fiber / sodium alginate three-dimensional precursor material.

[0030] (3) Using deionized water as solvent, prepare a 5% citric acid modified solution, add 0.1% concentrated sulfuric acid as catalyst to the modified solution, and 3 The banana core fiber / sodium alginate three-dimensional precursor material obtained above was immersed in 50 mL of the modified solution, and then the banana core fiber / sodium alginate three-dimensional precursor material immersed in the modified solution was freeze-dried. The freeze-dried material was heated at 100°C for 50 minutes and washed with water until neutral, finally obtaining a biomass fiber-based three-dimensional chromatography material.

[0031] The volume density of the prepared biomass fiber-based three-dimensional chromatography material is 7.2 mg / cm 3 The plastic deformation of cyclic compression in water is 7.2%, and the adsorption capacity for template protein lysozyme is 1080 mg / g. Example 2

[0032] A biomass fiber-based three-dimensional chromatography material and a preparation method thereof, comprising the following steps:

[0033] (1) The long banana core fibers were extracted from natural banana stems. A small cutting machine was used to cut the long banana core fibers into short pieces. Then, deionized water was used as the solvent and the long banana core fibers were dispersed by a shearing disperser. During the dispersion process, the speed of the shearing disperser was 5000 rpm and the dispersion time was 60 minutes. The fiber dispersion was then dried to obtain short banana core fibers with an average fiber length of 120 μm.

[0034] (2) A certain amount of banana core fiber staple fibers and sodium alginate were homogenously dispersed in deionized water to prepare a fiber dispersion, wherein the concentration of biomass staple fibers was 1.5% and the concentration of sodium alginate was 0.5%. The speed of the homogenizer during the dispersion process was 2000 rpm and the dispersion time was 50 minutes. The prepared fiber dispersion was poured into a mold and then freeze-dried at a freezing temperature of -80 °C and a vacuum degree of 10 Pa to obtain a banana core fiber / sodium alginate three-dimensional precursor material.

[0035] (3) Using deionized water as solvent, prepare a 10% citric acid modified solution, add 0.2% concentrated sulfuric acid as catalyst to the modified solution, and add 10cm 3 The banana core fiber / sodium alginate three-dimensional precursor material obtained above was immersed in 50 mL of the modified solution, and then the banana core fiber / sodium alginate three-dimensional precursor material immersed in the modified solution was freeze-dried. The freeze-dried material was heated at 110°C for 60 minutes and washed with water until neutral, finally obtaining a biomass fiber-based three-dimensional chromatography material.

[0036] The volume density of the prepared biomass fiber-based three-dimensional chromatography material is 28.6 mg / cm 3 The plastic deformation of cyclic compression in water is 3.9%, and the adsorption capacity for template protein lysozyme is 2300 mg / g. Example 3

[0037] A biomass fiber-based three-dimensional chromatography material and a preparation method thereof, comprising the following steps:

[0038] (1) The long banana core fibers were extracted from natural banana stems. A small cutting machine was used to cut the long banana core fibers into short pieces. Then, deionized water was used as the solvent and the long banana core fibers were dispersed by a shearing disperser. During the dispersion process, the speed of the shearing disperser was 8000 rpm and the dispersion time was 100 minutes. The fiber dispersion was then dried to obtain short banana core fibers with an average fiber length of 100 μm.

[0039] (2) A certain amount of banana core fiber staple fibers and sodium alginate were homogenously dispersed in deionized water to prepare a fiber dispersion, wherein the concentration of biomass staple fibers was 1.5% and the concentration of sodium alginate was 1%. The speed of the homogenizer during the dispersion process was 4000 rpm and the dispersion time was 10 minutes. The prepared fiber dispersion was poured into a mold and then freeze-dried at a freezing temperature of -80 °C and a vacuum degree of 10 Pa to obtain a banana core fiber / sodium alginate three-dimensional precursor material.

[0040] (3) Using deionized water as solvent, prepare a 10% citric acid modified solution, add 0.2% polyphosphoric acid as catalyst to the modified solution, and add 10cm 3 The banana core fiber / sodium alginate three-dimensional precursor material obtained above was immersed in 50 mL of the modified solution, and then the banana core fiber / sodium alginate three-dimensional precursor material immersed in the modified solution was freeze-dried. The freeze-dried material was heated at 115°C for 90 minutes and washed with water until neutral, finally obtaining a biomass fiber-based three-dimensional chromatography material.

[0041] The volume density of the prepared biomass fiber-based three-dimensional chromatography material is 32.3 mg / cm 3 The plastic deformation of cyclic compression in water is 4.7%, and the adsorption capacity for template protein lysozyme is 2800 mg / g.

Claims

1. A biomass fiber-based three-dimensional chromatography material, characterized in that: Prepared by the following steps: Step 1: extracting biomass fibers from natural plant stems and performing homogenization and dispersion treatment on the obtained biomass fibers to obtain biomass short fibers; The natural plant stems are banana stems, lotus stems or taro stems; In step 1, biomass fibers are extracted from the cross section of a natural plant stem using an extraction method; the homogenous dispersion treatment in step 1 is to disperse the biomass fibers in deionized water and then shear and disperse them, the speed of the shear disperser is 1000-10000 rpm, and the dispersion time is 30-120 minutes; the length of the biomass short fibers in step 1 is 10-200 μm; Step 2: homogeneously co-dispersing the biomass short fibers obtained in step 1 with natural high molecular weight polysaccharides to obtain a biomass fiber composite slurry, and then freeze-drying the composite slurry to obtain a biomass fiber three-dimensional precursor material; The natural high molecular weight polysaccharide is sodium alginate; In the biomass fiber composite slurry, the concentration of biomass short fibers is 0.1-5%, and the concentration of natural high molecular weight polysaccharides is 0.05-2%. The homogenization dispersion conditions in step 2 are 1000-5000 rpm and the dispersion time is 10-60 minutes; the freeze-drying conditions in step 2 are a temperature of -20--80°C and a vacuum degree of 1-100 Pa; Step 3, impregnating the precursor material obtained in step 2 in a modification solution, then freeze-drying the impregnated precursor material, heat-treating it after freeze-drying, and washing it with water until it is neutral, thereby obtaining a biomass fiber-based three-dimensional chromatography material; The modified solution is a mixed solution of citric acid and a catalyst, the concentration of citric acid is 0.1-20%, and the catalyst is concentrated sulfuric acid or polyphosphoric acid; The heat treatment temperature in step 3 is 90-140° C. and the time is 30-120 minutes.