WO2024025441A1

WO2024025441A1 - Method for integrated processing of meadow hay

Info

Publication number: WO2024025441A1
Application number: PCT/RU2023/050178
Authority: WO
Inventors: Михаил Викторович ИВАНОВ; Николай Петрович БРИЗИЦКИЙ
Original assignee: Михаил Викторович ИВАНОВ
Priority date: 2022-07-27
Filing date: 2023-07-21
Publication date: 2024-02-01

Abstract

The invention relates to the field of agriculture. Proposed is a method for the integrated processing of meadow hay, according to which hay is chopped and separated by pneumatic separation into a stalk fraction and a leaf fraction. The stalk fraction is cooked to obtain cellulose and cellulose-containing fibre. Leaf fraction having a protein content of more than 20% on a dry matter basis is sent for sequential processing, in a first step of which a lipid-pigment complex is obtained by maceration with ethanol, and in a second step of which a protein concentrate is obtained by three-step extraction with a solution of ammonium sulphate followed by precipitation. Meal obtained as a result of the sequential processing is sent to the cooking stage. Leaf fraction having a protein content of less than 20% on a dry matter basis is sent for pelleting or briquetting. The method provides for maximal recovery of useful products from non-wood feedstock.

Description

Method for complex processing of hay from meadow plants

TECHNICAL FIELD

The present invention relates to the field of agriculture, specifically, to the technology of complex processing of hay obtained from various types of meadow plants, which is aimed at the production of products useful in agriculture and other industries, such as cellulose and enriched animal feed, as well as others products intended for use in agriculture and other industries.

BACKGROUND OF THE ART

A source of information is known from the prior art that describes a method for producing a suspension based on herbal fibrous materials for the manufacture of sheets or slabs, which includes the following stages: collecting meadow grass; cleaning meadow grass mechanically or by blowing air and/or washing with water; cutting meadow grass to obtain a length from 100 to 0.1 mm; fibrillation grinding of meadow grass; making tablets from meadow grass; suspending meadow grass in water; adding fractions of cellulose fibers and/or paper waste and/or auxiliary substances to the suspension (EA 029141 B1, 02/28/2018).

A known source of information describes a method for separating components from plant material containing at least leaf and/or stem parts, wherein the material is at least partially defibrated and then separated into a fiber fraction and a sap stream so that that the fiber fraction mainly contains hard tissues, such as epidermis, sclerenchyma and vascular bundles, and the sap flow mainly contains soft tissues, such as parenchyma and cytosol (RU 2213169 C2, 09.27.2003).

There is a known source of information that describes a method for producing cellulose, including the use of non-wood plant raw materials with the content of native cellulose is not more than 50% and an aqueous solution of caustic soda, while the feedstock is washed with water at a temperature of 40 - 70 ° C and atmospheric pressure for 0.5 - 4 hours, delignification is carried out with an aqueous solution of nitric acid with a concentration of 2 - 8%, treatment is carried out at a temperature of 90 - 95 ° C for 4 - 20 hours, followed by separation of the solid phase and its further treatment with an aqueous solution of caustic soda with a concentration of 1 - 4%, at a temperature of 60 - 95 ° C for 1 - 6 hours, then the resulting The cellulose is filtered, washed with water and its moisture content is reduced (RU 2448118 C1, 04/20/2012).

The closest to the proposed technical solution is a source of information describing a continuous method for the production of cellulose pulp from herbaceous plant raw materials, including the following steps: preparation of herbaceous plant raw materials by grinding into pieces 1.5 - 30 cm long and 0.5 - 15 mm in diameter and removing dust particles from the specified raw materials using a fan; and continuous cooking of dust-free herbaceous plant raw materials, prepared earlier, in a cooking unit, which is a vertical column with smooth internal walls, into the upper part of which the conveyor continuously feeds herbaceous plant raw materials, while in parallel with the supply of dust-free raw materials to the upper part of the specified The digester is continuously supplied with cooking chemicals (a group consisting of NaOH and NaCl or NaiSCh), fresh water, reduced water and steam, the cooking temperature is 70 - 100°C, and during the continuous cooking process described, a suspension is formed with the following composition: weight percentage of NaOH 0.9 - 1.5, weight percentage of NaCl or NaiSOsOJS - 0.4; and the weight percentage of herbaceous plant materials is 15 - 18; where the concentration of ingredients is calculated from the weight of the liquid phase; The decomposition of non-cellulosic material from herbaceous plant materials occurs during the transition of the mass from the upper to the lower part of the specified digestion unit solely under the influence of gravity, which lasts from 40 minutes to 20 hours and the welded mass is concentrated in the lower part of the cooking unit and is continuously, at a speed equal to the feed speed, removed from the lower part of the cooking unit using a conveyor, which makes it possible to compensate for hydraulic pressure (RU 2636556 C1, 11/23/2017).

The main significant drawback of these inventions is the incomplete extraction of useful products (components) from non-wood plant materials.

DISCLOSURE OF INVENTION

The problem to be solved by the present invention is the development of a method for complex processing of hay from meadow plants, ensuring maximum extraction of useful products from it, including through the stage of preliminary fractionation of chopped hay into leaf and stem fractions.

The technical result achieved in solving the problem is the fullest possible extraction of useful products from non-wood plant raw materials, such as cellulose, cellulose-containing fibers, lipid-pigment complex and protein, as well as the production of enriched hay granules or briquettes intended for feeding farm animals, with a simultaneous reduction in the consumption of reagents, water, time, energy and ultimately reducing costs and improving the quality of cellulose.

IMPLEMENTATION OF THE INVENTION

To achieve the specified technical result, a method for complex processing of hay from meadow plants is proposed, according to which the hay is first crushed to a particle size of 10 - 30 mm (and this particle size is at least 80% of the total volume of hay) and separated by separation into stem and leaf fractions , after which the stem fraction is subjected to cooking to obtain cellulose in an amount of 20 - 50% of the amount of feedstock and cellulose-containing fiber from 1.2 - 20% from the amount of initial raw material, and the leaf fraction with a protein content of more than 20% in dry matter is sent for sequential processing, at the first stage of which a lipid-pigment complex is obtained by maceration with ethyl alcohol, at the second stage a concentrate is obtained by three-stage extraction with an ammonium sulfate solution followed by precipitation squirrel. The meal obtained as a result of sequential processing is sent to the cooking stage, and the leaf fraction with a protein content of less than 20% in dry matter is sent for granulation or briquetting to produce hay granulate or briquettes with a reduced fiber content.

In one embodiment of the invention, the hay is separated by air separation into stem and leaf fractions.

In addition, in one embodiment of the invention, the method is carried out without the stage of cooking the stem fraction.

It is also possible to add the resulting protein to the leaf fraction when producing granulates or hay briquettes with reduced fiber content to enrich it with protein.

Also, to solve the problem of effective processing of low-grade and substandard hay, it is possible to use hay with a crude fiber content of more than 30% of the total mass of hay as raw material.

The raw material for the implementation of the proposed method is meadow hay obtained from meadow plants.

The meadow is a complex plant community - a phytocenosis, the plants of which are represented mainly by perennial mesophytic grasses, that is, plants that require high moisture content for normal growth and development. Based on the nature of their origin, meadows are divided into natural meadows and artificial meadows. Natural meadows are covered with wild grasses, while artificial meadows are forage areas created by sowing perennial legumes and cereal forage grasses. All forage plants of meadows are divided in agricultural practice into four economic groups: cereals, legumes, sedges and forbs. The feeding value of meadows and herbaceous vegetation can be judged by the botanical composition, that is, the species composition of herbs. It determines the richness of the phytocenosis and affects the possibility of economic use of the meadow. Natural meadows formed in river valleys are considered the richest, where up to 80 plant species can grow per 1 ^m2 . Highly nutritious hay is obtained from perennial and annual legumes and cereal grasses in their pure form, from their mixtures, as well as from the grass of natural lands. Depending on the botanical composition and growing conditions of grasses, hay is classified as follows:

- seeded legumes (leguminous plants more than 60%);

- seeded cereals (cereals more than 60%, legumes less than 20%);

- seeded legumes and cereals (legumes from 20 to 60%);

- natural forage lands (cereals, legumes, forbs).

The most common methods of preserving green mass are drying them or storing them wet in an anaerobic and acidic environment. The first method is to prepare hay and artificially dried grass feed, the second is silage. Based on a combination of these two methods, haylage and wet hay are prepared.

Requirements for the quality of hay are regulated by the industry standard GOST 10243-2000.

The moisture content should be no more than 17%, the color of the hay should be from green to yellow-green and the smell characteristic of fresh hay.

Also applicable to hay is GOST R 55452-2013, which standardizes the following:

- mass fraction of crude protein in dry matter (%, not less): for bean hay of the 1st class - 15,

2nd - 13,

3rd - no less than 10%; cereal - 13%, 10% and 8%, respectively; seeded legumes and cereals - 14%, 11% and 9%; hay from natural hayfields - 11%, 9% and 7%;

- mass fraction of crude fiber in dry matter (%, no more): for seeded legume hay of the 1st class 28,

2nd - 30,

3rd - 31; sown cereals, respectively - 30%, 32% and 33%; seeded legumes and cereals - 29%, 31% and 32%; hay from natural hayfields 30%, 32% and 33%.

In this case, the most useful food is collected in the budding phase and the beginning of flowering. Overgrown grass reduces the quality of forage, and grass collected at the heading stage is generally substandard.

It is known that meadow grass hay is rich not only in fiber, but also in other useful components (proteins, fats, minerals); however, the qualitative and quantitative composition of the leaf and stem parts of the hay is not identical, and each of these parts is preferable for obtaining separate products ( the stem is cellulose, the leaves are protein), and therefore, it became necessary to separate the chopped hay into two fractions (leaf and stem).

From the studies conducted, it follows that dividing the feedstock into two fractions more than halves the content of lignin in the stem fraction from 60.38 to 26.56 and extractive substances from 1.47 to 0.65, which is important because, cellulose removal involves the removal of lignin and extractives. It is obvious that reducing the content of ballast substances will reduce the consumption of reagents, water, time, energy and ultimately reduce costs and improve the quality of cellulose.

The present invention is further disclosed by means of the following non-limiting example implementation.

An example of the method implementation. b Raw materials containing crude fiber from 16 to 36% of the total mass of hay and consisting of meadow plants are crushed to a particle size of 10 - 30 mm and sent to the stage of separation into two fractions: the heavy fraction (stems) and the light fraction (leaves). The separation process is carried out by the method of aeroseparation, using, for example, a ZIG-ZAG type aeroseparator with a capacity of 50 kg/h, with an upward air flow from 650 to 700 rpm. At the same time, a pattern has been established that due to the fact that the raw material is quite plastic and responds well to dynamic changes in the process, an increase in the upward air flow (650 rpm-700 rpm) ensures a change in the ratio of the stem/leaf fraction. This allows you to quickly respond to the technological needs of production. After obtaining the leaf and stem fractions, they are sent for further processing.

The resulting stem fraction is sent to the cooking stage. It should be noted that when implementing the proposed method, any cooking known from the prior art can be used: sulphate cooking, soda cooking, water hydrolysis, cooking with hydrogen peroxide. For example, cooking of the stem fraction using water hydrolysis technology is carried out at a temperature of about 170°C; the duration of standing at a given temperature is about 30 minutes, the duration of grinding is about 10 minutes. Peroxide cooking of the stem fraction without chelation is carried out according to the regime: NaOH consumption of about 20%, cooking temperature of about 140 °C; The duration of parking at a given temperature is about 180 minutes, the consumption of hydrogen peroxide is about 3 kg/t. Sulfate cooking of the stem fraction is carried out according to the following regime: consumption of active alkali, % of the feedstock about 12; cooking temperature about 150°C; the duration of standing at a given temperature is about 10 - 30 minutes, the duration of grinding before washing is about 2 minutes. It should be noted that the given process parameters are approximate and are selected depending on the quality and quantitative composition of the stem fraction. As a result of the cooking process, cellulose is obtained in an amount of 20 - 50% of the amount of the original raw material and cellulose-containing fiber in the amount of 1.2 - 20% of the amount of the original raw material. The resulting products can be used as independent products in agriculture and other industries, and can be further processed for additional processing, including the production of cellulose derivatives such as microcellulose, nanocellulose, or, for example, at the stage of grinding, washing, filtration and drying to produce paper/cardboard.

The resulting leaf fraction is sent for further processing depending on its protein content.

The leaf fraction with a protein content of more than 20% in dry matter is sent for sequential processing.

The following data were experimentally determined for the hay sample under study:

Extraction of the lipid-pigment complex and protein isolation are carried out by sequential processing of plant raw materials. At the first stage, a lipid-pigment complex is obtained by maceration with ethyl alcohol. Extraction is carried out in two stages of approximately 20 minutes each. In this case, ethyl alcohol is used as an extractant, the hydromodulus is 1:20, the process temperature is about 60°C, and the entire process time is about 40 minutes. The use of ethyl alcohol as an extractant is due to the fact that it most completely extracts the lipid-pigment complex. The yield of solid extract reaches 2.17%, which corresponds to 92% extraction of crude fat. After removal of the lipid-pigment complex, an increase in the crude protein content is observed from 3.1 to 3.24%. This fact is determined by the extraction of the non-protein part - the lipid-pigment complex - from the hay sample. Preliminary removal of the lipid-pigment complex with alcohols has a positive effect on the yield of protein concentrate (increases from 2.1% to 2.6-3%) and its quality (protein content in the concentrate increases from 19.5 to 20-23%) at the second stage process. The degree of protein extraction increases from 12.8% to 16-22% with preliminary maceration with alcohols.

Then, the treated hay is sent for three-stage protein extraction with ammonium sulfate solutions (0.5, 2.5, 5%, respectively). Ammonium sulfate solutions and raw materials were pre-cooled to 5°C, while the hydromodulus was 1:20, the extraction duration was about 15 minutes for each stage. In the resulting extract, the protein is in a colloidal dispersed state and for its precipitation it is necessary empirically determine the isoelectric point - the pH of zero charge of a colloidal particle. At the isoelectric point, agglomeration of protein globules and protein precipitation occurs. A 5% sulfuric acid solution was added to the protein solution in portions while controlling the pH and turbidity of the solution (turbidimetric titration). The pH value, which corresponds to the maximum value of the turbidity of the solution (the minimum value of the light transmittance coefficient - T, %), corresponds to an isoelectric point of 3.15 units. pH. To determine the turbidity (light transmittance) of the extract, a KFK-3 photoelectric colorimeter was used. At the same time, to precipitate protein from, for example, 300 ml of extract, it is necessary to spend 550 μl of a 5% sulfuric acid solution. The protein sediment (protein concentrate) is washed from ammonium sulfate with 10 ml of distilled water (until there is no ammonium ion in the washing water). The yield of protein concentrate was 2.1% of the initial mass of raw materials. The nitrogen content in the protein concentrate was 3.13%, which corresponds to a protein content of 19.5%. The degree of protein recovery was 12.8% of that present in the sample. The crude protein content after protein extraction was 2.7%, which is consistent with the protein recovery data. The protein isolated from the sample is “salt-soluble.” The protein present in plant materials can also be extracted by extraction with water (“water-soluble”) or alkali (“alkali-soluble”). Under similar conditions, a concentrate of “alkali-soluble” protein (0.05% sodium hydroxide solution) was isolated (RF Patent 2134991, 1999). Its yield was 0.29% with a nitrogen content of 16%, the degree of protein extraction was 1.5% of that present in the feedstock. For water-soluble protein, the yield of the concentrate was 0.21%, its nitrogen content was 25.8%, and the degree of protein extraction was 1.8% of the feedstock. In this case, the mechanical addition of the yields of protein fractions is incorrect, since, for example, a water-soluble fraction can be included in the alkali-soluble and salt-soluble protein fractions. In solution, after precipitation of the protein concentrate, an average organic carbon content of 840 mg/l was found, which corresponds to the extraction of BEV (in terms of starch) of 10.9% of the feedstock. The determination of organic carbon was carried out by high-temperature catalytic combustion using a total organic carbon analyzer TOC-L CSN (Shimadzu, Japan), while total organic carbon (TOC) is defined as the difference between total and inorganic carbon. The principle of determining total carbon (TC) is based on direct combustion of the sample in a specialized TC combustion tube filled with an oxidation catalyst and heated to 680°C. During combustion of the sample, all carbon is converted into carbon dioxide. Subsequently, the combustion products are determined in the cuvette of a non-dispersive infrared detector (NDIR). The method for determining inorganic carbon is based on measuring the carbon dioxide released into the gas phase when the acid reacts with carbonates and bicarbonates, and the total volume of carbon dioxide gas is measured by the same ND IR detector. Thus, it is possible to extract into concentrate up to 13% of the protein contained in the original raw material.

The meal obtained as a result of sequential processing is sent to the cooking stage, and then to the production of cellulose.

The leaf fraction with a protein content of less than 20% in dry matter is sent for granulation or briquetting. In this case, it is possible to use any known granulator or briquetting machine, which is selected taking into account production requirements. For briquetting grass cutting, for example, briquetting presses OKS-2, OPK-2, a press briquetting machine ПБШ-2 (stamp) and a ring-type briquetting machine designed by VIM are used. Granulated mass or briquettes are already valuable products in their own right. At the same time, the resulting granules or briquettes can be further enriched protein previously isolated from the protein-rich leaf fraction.

As a result of the implementation of the proposed method, cellulose, cellulose-containing fibers, a lipid-pigment complex, protein, enriched granules or briquettes are obtained, that is, the maximum extraction of useful substances from the hay of meadow plants is carried out.

Claims

Claim

1. A method for complex processing of hay from meadow plants, characterized by the fact that the hay is first crushed to a particle size of 10 - 30 mm and separated by separation into stem and leaf fractions, after which the stem fraction is subjected to cooking to obtain cellulose in an amount of 20 - 50% of the amount of feedstock and cellulose-containing fiber is from 1.2 - 20% of the amount of feedstock, and the leaf fraction with a protein content of more than 20% in dry matter is sent for sequential processing, at the first stage of which a lipid-pigment complex is obtained by maceration with ethyl alcohol, In the second stage, using a three-stage extraction method with ammonium sulfate solution followed by precipitation, a protein concentrate is obtained; the resulting sequential processing of the meal is sent to the cooking stage, and the leaf fraction with a protein content of less than 20% in dry matter is sent for granulation or briquetting to produce granulate or hay briquettes with low fiber content.

2. The method for complex processing of meadow hay according to claim 1, characterized in that the resulting protein was added to the leaf fraction during the production of hay granules or briquettes with low fiber content to enrich it with protein.

3. A method for complex processing of meadow hay according to claims 1-2, characterized in that hay with a crude fiber content of more than 30% of the total mass of hay is used as raw material.

4. The method for complex processing of meadow hay according to claim 1, characterized in that the hay is separated by air separation into stem and leaf fractions.

5. The method for complex processing of meadow hay according to claim 1, characterized in that the stem fraction is not subjected to cooking.