阅读说明：本技术 一种生物质纳米纤维素的制备方法 (Preparation method of biomass nanocellulose ) 是由 郝瑞文 谢文明 魏廉 于 2021-09-26 设计创作，主要内容包括：本发明公开了一种生物质纳米纤维素的制备方法,包括如下步骤：(1)HVP残渣的纯化：将HVP残渣和水分别计量加入物料缸中,持续搅拌,料水经离心分离得到纯化HVP残渣；(2)所述纯化HVP残渣的微粉化处理：所述纯化HVP残渣经液氮低温粉碎和冷冻干燥处理获得微米级粉体；(3)纳米纤维素悬浮液的制备：将所述微米级粉体配制成一定浓度的水性浆料,并添加适量的分散剂和研磨珠后经纳米砂磨机处理,得到所述纳米纤维素悬浮液；(4)纳米纤维素的制备：所述纳米纤维素悬浮液经冷冻干燥后得到粉体纳米纤维素。本发明提供一种绿色制备生物质纳米纤维素的方法,原料选自HVP残渣,可适合工业化大规模生产。(The invention discloses a preparation method of biomass nano-cellulose, which comprises the following steps: (1) purification of HVP residue: respectively metering HVP residues and water into a material jar, continuously stirring, and centrifugally separating the material water to obtain purified HVP residues; (2) micronization treatment of the purified HVP residue: carrying out liquid nitrogen low-temperature crushing and freeze drying treatment on the purified HVP residues to obtain micron-sized powder; (3) preparation of nanocellulose suspension: preparing the micron-sized powder into aqueous slurry with a certain concentration, adding a proper amount of dispersing agent and grinding beads, and treating the aqueous slurry by using a nano sand mill to obtain the nano cellulose suspension; (4) preparing nano-cellulose: and freeze-drying the nano-cellulose suspension to obtain the powdery nano-cellulose. The invention provides a green preparation method of biomass nano-cellulose, wherein the raw material is selected from HVP residues, and the method is suitable for industrial large-scale production.)

1. The preparation method of the biomass nanocellulose is characterized by comprising the following steps:

(1) purification of HVP residue: respectively metering HVP residues and water into a material jar, continuously stirring, and centrifugally separating the material water to obtain purified HVP residues;

(2) micronization treatment of the purified HVP residue: carrying out liquid nitrogen low-temperature crushing and freeze drying treatment on the purified HVP residues to obtain micron-sized powder;

(3) preparation of nanocellulose suspension: preparing the micron-sized powder into aqueous slurry with a certain concentration, adding a proper amount of dispersing agent and grinding beads, and treating the aqueous slurry by using a nano sand mill to obtain the nano cellulose suspension;

(4) preparing nano-cellulose: and freeze-drying the nano-cellulose suspension to obtain the powdery nano-cellulose.

2. The method for preparing biomass nanocellulose according to claim 1, wherein in step (1), the HVP residues are one or a combination of soybean meal HVP residues and corn meal HVP residues.

3. The method for preparing biomass nanocellulose according to claim 1, wherein in step (1), the weight ratio of the HVP residue to water is 1: 4.

4. The method for preparing biomass nanocellulose according to claim 1, wherein in step (3), the concentration of the aqueous slurry is 6 to 8%.

5. The method for preparing biomass nanocellulose according to claim 1, wherein in step (3), the dispersant added to the nanocellulose suspension is one of sodium hexametaphosphate, sodium pyrophosphate, sodium citrate and β -cyclodextrin.

6. The method according to claim 1, wherein in the step (3), the grinding beads are zirconia beads; the particle size range of the grinding beads is 0.2-0.4 mm.

7. The method for preparing biomass nanocellulose according to claim 1, wherein in step (3), the linear velocity of the grinding dispersion is 8 m/s.

8. The method according to claim 1, wherein the dispersant is added in an amount of 0.5 to 1% by dry weight of the HVP residue in the step (3).

9. The method for preparing biomass nanocellulose according to claim 1, wherein the purification of the HVP residue of step (1) is performed in triplicate.

10. The method for preparing biomass nanocellulose according to claim 1, wherein in step (3), the grinding time is 6-10 h.

Technical Field

The invention relates to the technical field of biomass nano-cellulose production, in particular to a preparation method of biomass nano-cellulose.

Background

In the food industry, Hydrolyzed Vegetable Protein (HVP) is a kind of hydrolysis product mainly made of soybean, corn or wheat Protein (mainly including one or more of acid hydrolysis, alkali hydrolysis and enzyme hydrolysis), and is widely used in the seasoning industry due to its taste characteristics mainly including umami taste. At present, protein raw materials of HVP mainly comprise soybean meal and corn meal, and the components of the soybean meal and the corn meal mainly comprise certain content of protein and certain amount of fiber components, so that no matter which hydrolysis process is carried out on the raw materials, the products of the raw materials also comprise the byproduct of HVP residues besides protein hydrolysate. Currently, HVP residues from various manufacturers are mainly treated as waste.

In recent years, with the deep knowledge of nanocellulose, nanocellulose has the advantages of good mechanical strength, high specific surface area, low thermal expansion coefficient and the like, and is widely applied to the fields of fine chemical engineering, composite materials, cosmetics, medicines and the like. Considering that the Hydrolyzed Vegetable Protein (HVP) residue contains a large amount of fiber components and partial residual amino acids and a small amount of water-soluble proteins, if the soluble and insoluble components are subjected to simple separation treatment, the residual amino acids and the small amount of water-soluble proteins can be effectively recovered, and simultaneously, the method provides feasibility for the application of the purified HVP residue in biomass nano-cellulose. At present, no report is found on the method and application of Hydrolyzing Vegetable Protein (HVP) residues to prepare biomass nano-cellulose.

Accordingly, those skilled in the art have been devoted to developing a method for preparing biomass nanocellulose using Hydrolyzed Vegetable Protein (HVP) residues.

Disclosure of Invention

In view of the above-mentioned drawbacks of the prior art, the technical problem to be solved by the present invention is how to prepare biomass nanocellulose from Hydrolyzed Vegetable Protein (HVP) residues.

In order to achieve the above object, the present invention provides a method for preparing biomass nanocellulose, comprising the following steps:

(1) purification of HVP residue: respectively metering HVP residues and water into a material jar, continuously stirring, and centrifugally separating the material water to obtain purified HVP residues;

(2) micronization treatment of the purified HVP residue: carrying out liquid nitrogen low-temperature crushing and freeze drying treatment on the purified HVP residues to obtain micron-sized powder;

(3) preparation of nanocellulose suspension: preparing the micron-sized powder into aqueous slurry with a certain concentration, adding a proper amount of dispersing agent and grinding beads, and treating the aqueous slurry by using a nano sand mill to obtain the nano cellulose suspension;

(4) preparing nano-cellulose: and freeze-drying the nano-cellulose suspension to obtain the powdery nano-cellulose.

Further, in the step (1), the HVP residues are one or a combination of two of soybean meal HVP residues and corn meal HVP residues.

Further, in the step (1), the weight ratio of the HVP residue to water is 1: 4.

Further, in the step (3), the concentration of the aqueous slurry is 6-8%.

Further, in the step (3), the dispersant added to the nanocellulose suspension is one of sodium hexametaphosphate, sodium pyrophosphate, sodium citrate and beta-cyclodextrin.

Further, in the step (3), the grinding beads are zirconia beads; the particle size range of the grinding beads is 0.2-0.4 mm.

Further, in the step (3), the linear velocity of the grinding dispersion was 8 m/s.

Further, in the step (3), the dispersant is added in an amount of 0.5 to 1% by dry weight of the HVP residue.

Further, the purification of the HVP residue of step (1) was repeated three times.

Further, in the step (3), the grinding time is 6-10 h.

The invention has at least the following beneficial technical effects:

1. the method successfully prepares the biomass nanocellulose from the HVP residues by adopting liquid nitrogen low-temperature crushing combined with a nano grinding dispersion technology, and expands a new raw material source for preparing the biomass nanocellulose;

2. the raw material source of the biomass nano-cellulose prepared by the invention is mainly byproduct HVP residues of hydrolyzed vegetable protein seasoning liquid manufacturers, so that the problem of troublesome subsequent treatment of the HVP residues is solved, and the strategic requirements of renewable resource development are met;

3. the preparation process is simple and safe, and is easy for industrial production;

4. the invention expands the application range of the soybean meal and the corn meal, and further improves the comprehensive utilization value of the soybean meal and the corn meal;

5. the invention is mainly a physical preparation technology, and meets the strategic requirements of national clean production.

The conception, the specific structure, and the technical effects produced by the present invention will be further described below to fully understand the objects, the features, and the effects of the present invention.

Detailed Description

The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.

Example 1

The invention provides a preparation method for preparing biomass nano-cellulose by utilizing soybean meal HVP (hydrolyzed vegetable protein) residues, which comprises the following steps:

(1) and (3) purifying and treating the soybean meal HVP residues: weighing 2kg of soybean meal HVP residues and 8kg of water, placing the residues and the 8kg of water in a material cylinder, continuously stirring for 0.5h, carrying out centrifugal separation on the material water to obtain a purified HVP soybean meal residue material, and repeating the steps (material water stirring and material water separation) for three times;

(2) micronization treatment of purified HVP soybean meal residue: carrying out liquid nitrogen low-temperature crushing and freeze drying on the purified HVP soybean meal residue material to obtain micron-sized powder with the particle size of more than 200 meshes;

(3) preparation of nanocellulose suspension: taking 120g of micron-sized powder, preparing 2000g of aqueous slurry with the concentration of 6%, adding 0.12g of sodium citrate dispersant, continuously stirring, and grinding the prepared aqueous slurry for 6 hours by a nano sand mill (0.2-0.4mm zirconium beads, linear velocity of 8m/s) to obtain nano cellulose suspension;

(4) preparing nano cellulose powder: and freeze-drying the nano-cellulose suspension to obtain the powder type nano-cellulose.

Example 2

The invention relates to a preparation method for preparing biomass nano-cellulose by utilizing corn meal HVP (hydrolyzed vegetable protein) residues, which comprises the following steps:

(1) and (3) purification treatment of corn meal HVP residues: weighing 2kg of corn meal HVP residues and 8kg of water, placing the residues and the 8kg of water in a material cylinder, continuously stirring for 0.5h, carrying out centrifugal separation on the material water to obtain a purified corn meal HVP residue material, and repeating the steps (material water stirring and material water separation) for three times;

(2) micronization treatment of HVP residue of purified corn meal: the purified HVP residue material is subjected to liquid nitrogen low-temperature crushing and freeze drying treatment to obtain micron-sized powder with the particle size of more than 200 meshes;

(3) preparation of nanocellulose suspension: taking 320g of micron-sized powder, preparing 4000g of aqueous slurry with the concentration of 8%, continuously stirring, adding 0.16g of sodium hexametaphosphate dispersant, and grinding the prepared aqueous slurry for 10 hours by a nano sand mill (0.2-0.4mm zirconium beads, linear velocity of 8m/s) to obtain nano cellulose suspension;

(4) preparing nano cellulose powder: and freeze-drying the nano-cellulose suspension to obtain the powder type nano-cellulose.

Example 3

The invention relates to a preparation method for preparing biomass nano-cellulose by utilizing corn meal HVP (hydrolyzed vegetable protein) residues, which comprises the following steps:

(1) and (3) purification treatment of corn meal HVP residues: weighing 2kg of corn meal HVP residues and 8kg of water, placing the residues and the 8kg of water in a material cylinder, continuously stirring for 0.5h, carrying out centrifugal separation on the material water to obtain a purified corn meal HVP residue material, and repeating the steps (material water stirring and material water separation) for three times;

(2) micronization treatment of HVP residue of purified corn meal: the purified HVP residue material is subjected to liquid nitrogen low-temperature crushing and freeze drying treatment to obtain micron-sized powder with the particle size of more than 200 meshes;

(3) preparation of nanocellulose suspension: preparing 2000g of 8% aqueous slurry from 160g of micron-sized powder, continuously stirring, adding 0.128g of sodium pyrophosphate dispersant, and grinding the prepared aqueous slurry for 7 hours by a nano sand mill (0.2-0.4mm zirconium beads, linear velocity 8m/s) to obtain nano cellulose suspension;

(4) preparing nano cellulose powder: and freeze-drying the nano-cellulose suspension to obtain the powder type nano-cellulose.

Example 4

The invention relates to a preparation method for preparing biomass nano-cellulose by utilizing soybean meal HVP (hydrolyzed vegetable protein) residues, which comprises the following steps:

(1) and (3) purifying and treating the soybean meal HVP residues: weighing 2kg of soybean meal HVP residues and 8kg of water, placing the residues and the 8kg of water in a material cylinder, continuously stirring for 0.5h, carrying out centrifugal separation on the material water to obtain a purified HVP soybean meal residue material, and repeating the steps (material water stirring and material water separation) for three times;

(2) micronization treatment of purified HVP soybean meal residue: carrying out liquid nitrogen low-temperature crushing and freeze drying on the purified HVP soybean meal residue material to obtain micron-sized powder with the particle size of more than 200 meshes;

(3) preparation of nanocellulose suspension: preparing 2000g of water-based slurry with the concentration of 7% by taking 140g of micron-sized powder, adding 0.14g of beta-cyclodextrin dispersing agent, continuously stirring, and grinding the prepared water-based slurry for 8 hours by a nano sand mill (0.2-0.4mm zirconium beads, linear velocity of 8m/s) to obtain nano cellulose suspension;

(4) preparing nano cellulose powder: and freeze-drying the nano-cellulose suspension to obtain the powder type nano-cellulose.

Example 5

The invention relates to a preparation method for preparing biomass nano-cellulose by utilizing soybean meal and corn meal HVP (hydrolyzed vegetable protein) residues, which comprises the following steps:

(1) purification treatment of HVP residue: sequentially weighing 1kg of soybean meal HVP residues, corn meal HVP residues and 8kg of water, placing the materials in a material cylinder, continuously stirring for 0.5h, centrifugally separating the materials and the water to obtain a purified HVP soybean meal residue material, and repeating the steps (material-water stirring and material-water separation) for three times;

(2) micronization treatment of purified HVP residue: the purified HVP residue material is subjected to liquid nitrogen low-temperature crushing and freeze drying treatment to obtain micron-sized powder with the particle size of more than 200 meshes;

(3) preparation of nanocellulose suspension: preparing 150g of micron-sized powder into 2000g of aqueous slurry with the concentration of 7.5%, adding 0.15g of sodium citrate dispersant, continuously stirring, and grinding the prepared aqueous slurry for 10 hours by a nano sand mill (0.2-0.4mm zirconium beads, linear velocity of 8m/s) to obtain nano cellulose suspension;

(4) preparing nano cellulose powder: and freeze-drying the nano-cellulose suspension to obtain the powder type nano-cellulose.

As can be seen from examples 1-5, the obtained nanocellulose had a diameter of 15 to 75nm and a length of 150 to 1500 nm.

The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.