阅读说明：本技术 一种食品级微晶纤维素的制备方法及其应用 (Preparation method and application of food-grade microcrystalline cellulose ) 是由 叶有明 符舒娜 杨少辉 农永萍 谢雪珍 吴国勇 蒋才云 蓝峻峰 于 2019-10-10 设计创作，主要内容包括：本发明公开一种食品级微晶纤维素的制备方法,按如下步骤进行：(1)粉碎蔗渣：将榨糖后的甘蔗渣真空低温烘干,搅碎成粉末；(2)脱糖；(3)防变色处理：向所述滤渣Ⅰ加入酸性混合液,搅拌均匀、浸泡、甩干,得到滤渣Ⅱ,所述酸性混合液由乙酸、抗坏血酸和柠檬酸溶液组成；(4)漂白处理(5)酸解(6)后处理：将所述酸解后的物料进行甩干,并用热水浸泡,再用热水洗涤至中性,接着甩干、冷冻烘干、粉碎后,即得到食品级微晶纤维素产品。本发明方法具有产率高、颜色天然、不易变色、食用安全的优点,采用此方法制备出的饼干可延长饼干的保质期,可降低饼干的热量,调节人体膳食结构。(The invention discloses a preparation method of food-grade microcrystalline cellulose, which comprises the following steps of (1) crushing bagasse, drying the bagasse after sugar pressing at low temperature in vacuum, stirring the bagasse into powder, (2) desugaring, and (3) performing anti-discoloration treatment, namely adding acidic mixed liquid into the filter residue I, uniformly stirring, soaking and drying to obtain filter residue II, wherein the acidic mixed liquid consists of acetic acid, ascorbic acid and citric acid solution, and (4) bleaching treatment (5) performing acidolysis treatment (6) post-treatment, namely drying the acidolyzed material, soaking the material in hot water, washing the material to be neutral by using hot water, drying, freezing, drying and crushing to obtain a food-grade microcrystalline cellulose product.)

The preparation method of food-grade microcrystalline cellulose is characterized by comprising the following steps of:

(1) crushing bagasse: drying sugar-pressed bagasse at low temperature in vacuum, and crushing into powder;

(2) and (3) desugarizing: soaking the powder obtained in the step (1) in ethanol, and drying by spin-drying to obtain filter residue I;

(3) and (3) anti-discoloration treatment: adding an acidic mixed solution into the filter residue I, uniformly stirring, soaking and spin-drying to obtain a filter residue II, wherein the acidic mixed solution is composed of acetic acid, ascorbic acid and a citric acid solution;

(4) bleaching treatment: adding a sodium hydroxide solution into the filter residue II, heating, soaking, spin-drying and washing simultaneously to obtain a filter residue III;

(5) acid hydrolysis: adding hydrochloric acid into the filter residue III, heating to boil, preserving heat, standing, and spin-drying;

(6) and (3) post-treatment: and (3) spin-drying the acidolyzed material, soaking the material in hot water, washing the material to be neutral by using the hot water, spin-drying, freezing, drying and crushing the material to obtain the food-grade microcrystalline cellulose product.

2. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: the vacuum low-temperature drying is carried out, wherein the temperature is 60-70 ℃, the vacuum degree is-0.08-0.10 MPa, and the vacuum low-temperature drying time is 1-2 h; the particle size of the powder is 10-40 meshes.

3. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: in the step (2), the mass concentration of the ethanol is 20-40%, the mass-to-liquid ratio of the bagasse powder to the ethanol is 1: 1, and the soaking time is 2-3 hours.

4. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: in the step (3), the mass-to-solid-to-liquid ratio of the filter residue I after desugarization to the acidic mixed solution is 1: 2-4; in the acidic mixed solution, the mixing mass ratio of acetic acid, ascorbic acid and citric acid is 1: 1, the mass concentration of the acetic acid is 3-5%, the mass concentration of the ascorbic acid is 5-10%, and the mass concentration of the citric acid is 5-10%; the soaking time is 5-10 h.

5. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: in the step (4), the mass-to-solid-to-liquid ratio of the filter residue II obtained by the discoloration prevention treatment to the sodium hydroxide solution is 1: 3-5, the mass concentration of the sodium hydroxide is 5% -10%, the heating and soaking temperature is 80-90 ℃, and the soaking time is 1-2 hours; and the drying and the washing are carried out simultaneously, namely the filter residue II after being heated and soaked is washed while being dried by water for multiple times.

6. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: in the step (5), the mass liquid-solid ratio of the filter residue III obtained after bleaching to hydrochloric acid is 1: 3-5, the mass concentration of the hydrochloric acid is 3-4 mol/L, the heat preservation time is 1-1.5 hours, and the standing time is 24 hours.

7. The method of preparing food grade microcrystalline cellulose of claim 1, wherein: in the step (6), the temperature of the hot water is 90-100 ℃, and the time for soaking in the hot water is 15-30 min; the temperature of the freezing and drying is-20 ℃ to-30 ℃, and the time is 1-2 h; the crushed granularity is 80-100 meshes.

Use of food grade microcrystalline cellulose, characterized in that the food grade microcrystalline cellulose is used for making biscuits, the food grade microcrystalline cellulose being made by the method of any of claims 1-7 to .

9. The application of claim 8, wherein the biscuit comprises the raw materials of white sugar, milk powder, salt, baking soda, food-grade microcrystalline cellulose, edible oil, water and high gluten flour in a mass ratio of 15% to 5% to 0.5% to 1% to 3% to 5% to 10% to 25% in sequence.

Technical Field

The invention belongs to the field of microcrystalline cellulose preparation, and particularly relates to a preparation method and application of food-grade microcrystalline cellulose.

Background

China is the third largest sugarcane planting country in the world, and is second to India and Brazil, West is the most province for planting and producing cane sugar, sugarcane is an important economic crop and plays an important role in national economy, and the sugarcane contains more natural high molecular substances such as cellulose, hemicellulose, lignin and the like.

At present, there are chemical and enzymatic processes mainly used for the preparation of microcrystalline cellulose.

For example, lake Zhou Wang Tianming pharmaceutical company in Chinese patent application 201510034313.3 discloses a preparation method of microcrystalline cellulose, which comprises the steps of acidolysis, neutralization, filter pressing and washing, wherein the preparation method successfully prepares microcrystalline cellulose products, Beijing Peng Shengtian cellulose technology Limited company in Chinese patent application 201210290177.0 discloses a preparation method of microcrystalline cellulose, which adopts waste residues generated in the production process of xylitol as raw materials to prepare microcrystalline cellulose, and Dalian ocean university in Chinese patent application 201611099435.1 discloses which adopts fresh brown algae or brown algae residues to prepare kelp microcrystalline cellulose.

The enzymatic hydrolysis method has high specificity of , mild conditions, and is also a new methods for preparing microcrystalline cellulose, for example, methods for preparing microcrystalline cellulose by using crop straws are disclosed in China patent application 200910030244.3 of Jiangnan university.

The invention adopts biomass raw materials to prepare microcrystalline cellulose, and because sugar cane is easy to turn brown in the preparation process, bleaches which are harmful to human bodies, such as hydrogen peroxide, sodium chlorite, 1, 3-dimethyl-2-imidazolidinone, 3-methyl-1-butyl pyrrole chloride and the like, are used, and because the microcrystalline cellulose has large pores and is loose, the bleaches are easy to remain in the microcrystalline cellulose and are difficult to clean.

201611238112.6, the name of the invention is , the method comprises the steps of pretreating a plant fiber raw material by adopting an organic solvent or an organic solvent aqueous solution to obtain a pretreated plant fiber raw material and a pretreatment solution, cooking the pretreated plant fiber raw material by adopting the organic solvent or the organic solvent aqueous solution as a cooking solvent and adding a catalyst, carrying out solid-liquid separation on the pretreated plant fiber raw material to obtain a cooking solution and fibers, and carrying out bleaching treatment, water washing treatment, drying treatment and crushing treatment on the obtained fibers to obtain the microcrystalline cellulose.

Disclosure of Invention

The invention aims to solve the technical problems and provides food-grade microcrystalline cellulose preparation methods which are high in yield, natural in color, difficult to discolor and safe to eat.

In order to achieve the purpose, the technical scheme of the invention is as follows:

the preparation method of food-grade microcrystalline cellulose comprises the following steps:

(1) crushing bagasse: drying sugar-pressed bagasse at low temperature in vacuum, and crushing into powder;

(2) and (3) desugarizing: soaking the powder obtained in the step (1) in ethanol, and drying by spin-drying to obtain filter residue I;

(3) and (3) anti-discoloration treatment: adding an acidic mixed solution into the filter residue I, uniformly stirring, soaking and spin-drying to obtain a filter residue II, wherein the acidic mixed solution is composed of acetic acid, ascorbic acid and a citric acid solution;

(4) bleaching treatment: adding a sodium hydroxide solution into the filter residue II, heating, soaking, spin-drying and washing simultaneously to obtain a filter residue III;

(5) acid hydrolysis: adding hydrochloric acid into the filter residue III, heating to boil, preserving heat, standing, and spin-drying;

(6) and (3) post-treatment: and (3) spin-drying the acidolyzed material, soaking the material in hot water, washing the material to be neutral by using the hot water, spin-drying, freezing, drying and crushing the material to obtain the food-grade microcrystalline cellulose product.

The step is carried out by vacuum low-temperature drying at the temperature of 60-70 ℃, the vacuum degree of-0.08-0.10 MPa, the vacuum low-temperature drying time of 1-2h, and the particle size of the powder is 10-40 meshes.

As a technical scheme of the step , in the step (2), the mass concentration of the ethanol is 20% -40%, the mass-to-solid-to-liquid ratio of the bagasse powder to the ethanol is 1: 1, and the soaking time is 2-3 hours.

According to the technical scheme of the step , in the step (3), the mass-to-solid-to-liquid ratio of filter residue I after desugaring to the acid mixed solution is 1: 2-4, the mixed mass ratio of acetic acid, ascorbic acid and citric acid in the acid mixed solution is 1: 1, the mass concentration of acetic acid is 3-5%, the mass concentration of ascorbic acid is 5-10%, the mass concentration of citric acid is 5-10%, and the soaking time is 5-10 hours.

According to the technical scheme of the step, in the step (4), the mass solid-liquid ratio of the filter residue II obtained through the anti-discoloration treatment to a sodium hydroxide solution is 1: 3-5, the mass concentration of the sodium hydroxide is 5% -10%, the heating and soaking temperature is 80-90 ℃, the soaking time is 1-2 hours, and the filter residue II after heating and soaking is washed while being spun dry for multiple times.

According to the technical scheme of the step, in the step (5), the mass liquid-solid ratio of filter residue III obtained after bleaching to hydrochloric acid is 1: 3-5, the mass concentration of the hydrochloric acid is 3-4 mol/L, the heat preservation time is 1-1.5 hours, and the standing time is 24 hours.

As a technical scheme for the step , in the step (6), the temperature of hot water is 90-100 ℃, the time of hot water soaking is 15-30 min, the temperature of freezing and drying is-20-30 ℃, the time is 1-2h, and the granularity of crushing is 80-100 meshes.

use of food grade microcrystalline cellulose for making biscuits, said food grade microcrystalline cellulose being made by the method of making as described above.

steps, wherein the raw materials of the biscuit comprise white sugar, milk powder, salt, baking soda, food-grade microcrystalline cellulose, edible oil, water and high gluten flour, and the mass ratio is 15 to 5 to 0.5 to 1 to 3 to 5 to 10 to 25.

Compared with the prior art, the invention has the beneficial effects that:

1. the invention adopts three anti-oxidation processes, wherein, the vacuum low-temperature drying is carried out on the bagasse before desugarization, thus effectively controlling the oxidation discoloration of the bagasse, the second anti-discoloration process is added between desugarization and bleaching, because researches show that the reason for the brown color of the sugarcane in the processing process is that polyphenol oxidase in the sugarcane oxidizes o-biphenol into o-benzoquinone, and the o-benzoquinone rapidly polymerizes to generate a brownish black pigment.

2. According to the invention, bagasse is soaked by ethanol, lignin in raw materials is removed in the aspect of , and cellulose can be degraded in the aspect of , so that the polymerization degree of the cellulose meets the product requirement of microcrystalline cellulose, the use of strong acid is reduced, and the generation of acidic wastewater is reduced.

3. The invention avoids using bleaching agents such as hydrogen peroxide, sodium chlorite, 1, 3-dimethyl-2-imidazolidinone, 3-methyl-1-butyl pyrrole chloride and the like which are harmful to human bodies, obtains the pure natural primary-color microcrystalline cellulose with the yield of more than 70 percent and the purity of more than 95 percent, and can be used as an additive in food.

4. The microcrystalline cellulose is used in the preparation of the biscuit and used as a stabilizer in the biscuit, so that the quality guarantee period of the biscuit is prolonged, the heat of the biscuit can be reduced, and the dietary structure of a human body is adjusted.

Detailed Description

The present invention is described in further detail with reference to the following examples, but the embodiments of the present invention are not limited to the scope of the examples.