CN115434175A - Method for synchronously recycling multiple active components from decomposed product covered by alkali heat treatment film - Google Patents
Method for synchronously recycling multiple active components from decomposed product covered by alkali heat treatment film Download PDFInfo
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- CN115434175A CN115434175A CN202211234960.5A CN202211234960A CN115434175A CN 115434175 A CN115434175 A CN 115434175A CN 202211234960 A CN202211234960 A CN 202211234960A CN 115434175 A CN115434175 A CN 115434175A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
Abstract
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for synchronously recycling multiple active components from a decomposition product covered by an alkali heat treatment film. The invention leads cellulose substances in the film covering decomposition products to be softened and expanded through alkali heat treatment, cuts off hydrogen bond connection between hemicellulose and cellulose, leads the cellulose substances and non-cellulose components to be separated, and promotes the precipitation and recovery of the cellulose and the hemicellulose. Meanwhile, carboxyl and phenolic hydroxyl on a humic acid structure in the film-covered humified product have weak acidity, and can perform a replacement reaction with an alkali extractant to form soluble humate, so that the dissolution recovery of the humic acid is improved. In addition, the alkali extractant solution adopted by the invention has lower mass concentration, can effectively prevent high-concentration alkali liquor from degrading dissolved hemicellulose and cellulose to form monosaccharide or polysaccharide, does not damage active components in the recovery process, and is beneficial to the recovery of cellulose and hemicellulose.
Description
Technical Field
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for synchronously recycling multiple active components from a decomposition product covered by an alkali heat treatment film.
Background
The film covering fermentation technology combines the molecular nano-film technology with the static aerobic composting technology, so that the high-temperature time of a compost is effectively prolonged, the composting is accelerated, meanwhile, the odor concentration can be reduced by 90-97%, and the cost for producing each ton of organic fertilizer by applying the film covering fermentation technology is less than 20 yuan. The rotten product after the film covering fermentation usually contains more than 45% of organic matters and can be used as an organic fertilizer, but the organic fertilizer is difficult to popularize due to poor fertilizer effect and low public acceptance. The film-covered humified products usually contain rich active components such as cellulose, hemicellulose, humic acid and the like, can be used for repairing polluted soil fields, preparing degradable films, medicine-carrying coatings and the like after being recovered, and have high application value and wide prospect. However, these active ingredients are often mixed in the humified products and cannot be directly utilized due to being wrapped by cell walls, and thus, the active ingredients can be recycled and recycled after being treated to a certain extent.
At present, the method for recovering cellulose, hemicellulose and humic acid from multi-element biomass waste raw materials such as agricultural straws, brewed fermented products and the like and fermentation products mainly comprises a mixed liquid extraction method of normal temperature and strong alkali and strong acid or an oxidant, such as a nitric acid-ethanol method, a sodium hydroxide-hydrogen peroxide method, a formic acid-acetic acid-hydrogen peroxide method, a sodium hydroxide-sodium hypochlorite-acetic acid method and the like. However, in the prior art, high-concentration alkali liquor is mainly used for respectively extracting active components such as cellulose, hemicellulose, humic acid and the like in multi-component organic waste at normal temperature, single active component is recovered, other active components are easily damaged by high-concentration alkali in the recovery process, and synchronous recovery of multiple active components cannot be realized.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for simultaneously recovering multiple active components from a film-covered humified product by alkali-heat treatment, wherein the method provided by the present invention can simultaneously recover cellulose, hemicellulose and humic acid in the film-covered humified product.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for synchronously recovering multiple active components from a film-covered rotting product by alkali heat treatment, which comprises the following steps:
mixing the film covered decomposed product with an alkali extractant solution, and performing alkali heat treatment to obtain an alkali heat treatment mixture; the mass concentration of the alkali extractant solution is 0.25-1.25%;
carrying out first solid-liquid separation on the alkali heat treatment mixture to respectively obtain a first solid and a supernatant;
washing the first solid until the pH value of the washing liquid is 7.2-8.2, and then carrying out first drying to obtain cellulose;
adjusting the pH value of the supernatant to 1-1.5, sequentially performing first standing and second solid-liquid separation to respectively obtain filtrate and a second solid, and performing second drying on the second solid to obtain humic acid;
and mixing the washing liquid with the filtrate, adjusting the pH value of the mixed liquid obtained by mixing to 5.5-7.5, adding absolute ethyl alcohol, sequentially performing second standing and third solid-liquid separation to obtain a third solid, and performing third drying on the third solid to obtain hemicellulose.
Preferably, the alkali extractant solution comprises an alkali metal hydroxide solution or ammonia.
Preferably, the mass ratio of the dry weight of the film covered humified product to the alkali extractant solution is 1:6-15.
Preferably, the temperature of the alkali heat treatment is 90-95 ℃, and the time is 90-120 min.
Preferably, the reagent for adjusting the pH of the supernatant comprises an inorganic acid solution.
Preferably, the reagent for adjusting the pH of the mixed solution includes an alkali metal hydroxide solution and/or an alkali metal carbonate solution.
Preferably, the temperatures of the first drying, the second drying and the third drying are independently 40 to 50 ℃.
Preferably, the first solid-liquid separation comprises centrifugation and filtration which are sequentially carried out; the speed of the centrifugation is 4000-8000 rpm, and the time is 5-10 min.
Preferably, the particle size of the film covered humified product is 0.18-0.28 mm.
The invention provides a method for synchronously recovering multiple active components from a film-covered rotting product by alkali heat treatment, which comprises the following steps: mixing the film covered decomposed product with an alkali extractant solution, and performing alkali heat treatment to obtain an alkali heat treatment mixture; the mass concentration of the alkali extractant solution is 0.25-1.25%; carrying out first solid-liquid separation on the alkali heat treatment mixture to respectively obtain a first solid and a supernatant; washing the first solid until the pH value of the washing liquid is 7.2-8.2, and then carrying out first drying to obtain cellulose; adjusting the pH value of the supernatant to 1-1.5, sequentially performing first standing and second solid-liquid separation to respectively obtain filtrate and a second solid, and performing second drying on the second solid to obtain humic acid; and mixing the washing liquid with the filtrate, adjusting the pH value of the mixed liquid obtained by mixing to 5.5-7.5, adding absolute ethyl alcohol, sequentially performing second standing and third solid-liquid separation to obtain a third solid, and performing third drying on the third solid to obtain hemicellulose.
The invention extracts active components in the fermentation product covered by the membrane by coupling alkali extraction and heat treatment, the heat treatment can soften and expand cellulose substances in the humified product covered by the membrane through high temperature, improve the solubility of humate, and untie the cross-linking structure of cellulose and hemicellulose molecular chains under the action of alkali extractant solution, cut off the hydrogen bond connection between the hemicellulose and the cellulose, reduce the polymerization degree and the crystallinity of the cellulose, and lead the cellulose to beSeparating substances from non-cellulose components, and promoting the precipitation and recovery of cellulose and hemicellulose. Meanwhile, carboxyl and phenolic hydroxyl on a humic acid structure in the film-covered humified product have weak acidity, and the humic acid and an alkali extracting agent undergo a displacement reaction to form soluble humate, so that the dissolution and recovery of the humic acid are improved. In addition, in the process of extracting cellulose and hemicellulose by using an alkali solution, the humic acid extracted synchronously can be used as a catalyst to accelerate the breakage of cell walls and promote the dissolution of the cellulose and the hemicellulose. Thereby realizing the synchronous recovery of cellulose, hemicellulose and humic acid multi-active components in the covering humified products through alkali treatment. In addition, the mass concentration (0.25-1.25 wt.%) of the alkali extractant solution adopted in the invention is lower than that of the high-concentration alkali liquor (6.00-9.00 wt.%) adopted in the prior art, so that OH extracted from the alkali liquor under high concentration can be effectively avoided - The concentration is increased, so that the dissolved hemicellulose and cellulose are degraded to form monosaccharide or polysaccharide, the amount of the degraded hemicellulose and cellulose is more than the dissolved amount of the cellulose and hemicellulose, active components cannot be damaged in the recovery process, and the extraction of the cellulose and the hemicellulose is facilitated.
In addition, the method for synchronously recycling the multiple active components from the products of film covering decomposition provided by the invention has the advantages of high extraction speed and short time consumption, and can realize synchronous and efficient recycling of the multiple active components from the products of film covering fermentation. The results of the examples show that the cellulose recovery rate is 27.29 to 31.56%, the hemicellulose recovery rate is 17.59 to 18.17%, and the humic acid recovery rate is 8.83 to 9.23%. The multi-active component recovered by the method provided by the invention can be used for the development of degradable membranes, drug-loaded coatings and soil pollution remediation agents, and has a wide application prospect.
Drawings
FIG. 1 is a flow chart of the method for covering the rotten product by the alkaline heat treatment film and synchronously recovering multiple active components;
FIG. 2 is a diagram of the film covering decomposition products before and after the alkali heat treatment, wherein A is the film covering decomposition products, and B is the mixture containing the active components after the alkali heat treatment;
FIG. 3 is a graph of the amount of active components in the humic product covered by the recovery film of different concentrations of alkali extractant solution at 90 ℃.
Detailed Description
The invention provides a method for synchronously recovering multiple active components from a film-covered rotting product by alkali heat treatment, which comprises the following steps:
mixing the film covered decomposed product with an alkali extractant solution, and performing alkali heat treatment to obtain an alkali heat treatment mixture; the mass concentration of the alkali extractant solution is 0.25-1.25%;
carrying out first solid-liquid separation on the alkali heat treatment mixture to respectively obtain a first solid and a supernatant;
washing the first solid until the pH value of the washing liquid is 7.2-8.2, and then carrying out first drying to obtain cellulose;
adjusting the pH value of the supernatant to 1-1.5, sequentially performing first standing and second solid-liquid separation to respectively obtain filtrate and a second solid, and performing second drying on the second solid to obtain humic acid;
and mixing the washing liquid with the filtrate, adjusting the pH value of the mixed liquid obtained by mixing to 5.5-7.5, adding absolute ethyl alcohol, sequentially performing second standing and third solid-liquid separation to obtain a third solid, and performing third drying on the third solid to obtain hemicellulose.
Unless otherwise specified, the present invention does not require any particular source of the raw materials used, and commercially available products known to those skilled in the art may be used.
The invention mixes the film covering humification product and the alkali extraction agent solution for alkali heat treatment.
In the present invention, the particle diameter of the film-covered humified product is preferably 0.18 to 0.28mm, and more preferably 0.21 to 0.25mm. The source of the film-covered humification product is not particularly limited in the present invention, and the film-covered humification product of a source well known in the art can be used. In the embodiment of the invention, the preparation process of the film covering decomposition product specifically comprises the following steps: livestock and poultry manure and crop straws with the mass ratio of 1:1 are taken as raw materials, and are fermented for 30D under the condition that the semi-permeable membrane is prepared by wrapping expanded polytetrafluoroethylene by two layers of 600D oxford fabric; the water content of the livestock and poultry manure is preferably 65-85%, and more preferably 70-80%; the water content of the crop straws is preferably 10-20%, and more preferably 10-15%; the two layers of 600D oxford cloth sandwich expanded polytetrafluoroethylene are commercially available goods.
The raw material adopted by the invention is a film-covered rotten product, and compared with a biomass waste raw material and a traditional fermentation product, the film-covered rotten product has higher active components such as cellulose, hemicellulose, humic acid and the like and higher recovery value.
Before the alkaline heat treatment, the film covering decomposition product is preferably subjected to pretreatment; the pretreatment preferably comprises drying, impurity removal, crushing and screening which are sequentially carried out; the drying is preferably air-drying under natural conditions; the impurity removal is preferably carried out by mechanical or manual sorting; the crushing equipment is preferably a crusher; the screening is preferably carried out using a 50-80 mesh screen, more preferably 60-70 mesh. The invention removes impurities such as stones, big clods, plastics and the like in the film covering rotten products by impurity removal.
In the present invention, the alkali extractant solution preferably includes an alkali metal hydroxide solution or aqueous ammonia, and the alkali metal hydroxide solution preferably includes a potassium hydroxide solution or a sodium hydroxide solution, more preferably a potassium hydroxide solution; the mass concentration of the alkali extractant solution is 0.25-1.25%, preferably 0.5-1%; the mass ratio of the dry weight of the film covered humus products to the alkali extractant solution is preferably 1:6-15, more preferably 1:7-10.
Compared with the high-concentration alkali liquor (6.00-9.00 wt.%) adopted in the prior art, the mass concentration of the alkali extractant solution adopted by the invention is lower, so that the OH extracted from the alkali liquor under high concentration can be effectively avoided - The concentration is increased, so that the dissolved hemicellulose and cellulose are degraded to form monosaccharide or polysaccharide, the amount of the degraded hemicellulose and cellulose is more than the dissolved amount of the cellulose and hemicellulose, and the extraction of the cellulose and the hemicellulose is not facilitated.
In the present invention, the temperature of the alkali heat treatment is preferably 90 to 95 ℃, more preferably 90 to 93 ℃, and the time is preferably 90 to 120min, more preferably 110 to 120min; the alkali heat treatment is preferably carried out under stirring. The stirring process is not particularly limited in the present invention, and a stirring process well known in the art may be used.
In the process of alkali heat treatment, cellulose substances in the film covering decomposed products are softened and expanded, the cross-linked structures of cellulose and hemicellulose molecular chains are untied under the action of an alkali extracting agent solution, hydrogen bond connection between the hemicellulose and the cellulose is cut off, the degree of polymerization and the crystallinity of the cellulose are reduced, the cellulose substances and non-cellulose components are separated, and the precipitation and recovery of the cellulose and the hemicellulose are promoted. Meanwhile, carboxyl and phenolic hydroxyl on a humic acid structure in the film-covered humified product have weak acidity, and the humic acid and an alkali extracting agent undergo a displacement reaction to form soluble humate, so that the dissolution recovery of the humic acid is improved. In addition, in the process of extracting cellulose and hemicellulose by using an alkali solution, the humic acid extracted synchronously can be used as a catalyst to accelerate the breakage of cell walls and promote the dissolution of the cellulose and the hemicellulose.
After the alkali heat treatment mixture is obtained, the alkali heat treatment mixture is subjected to first solid-liquid separation to respectively obtain a first solid and a supernatant.
In the present invention, the first solid-liquid separation preferably includes centrifugation and filtration performed in this order; the speed of the centrifugation is preferably 4000 to 8000rpm, more preferably 4000 to 6000rpm, and the time is preferably 5 to 10min, more preferably 8 to 10min. The filtration method is not particularly limited in the present invention, and a filtration method known in the art may be used.
Before the first solid-liquid separation is carried out, the present invention preferably cools the alkali-heat treated mixture to room temperature; the cooling is preferably natural cooling.
After the first solid is obtained, the first solid is washed until the pH value of the washing liquid is 7.2-8.2, and the washed first solid is obtained.
In the present invention, the pH of the washing solution is preferably 7.5 to 7.8; the washing process is preferably washing by using deionized water; the number of washing is preferably 4 to 8, more preferably 6 to 8.
After the washed first solid is obtained, the washed first solid is subjected to first drying to obtain the cellulose.
In the present invention, the temperature of the first drying is preferably 40 to 50 ℃, more preferably 45 to 50 ℃, and the time is preferably 12 to 16 hours, more preferably 12 to 15 hours; the drying is preferably oven drying.
After the supernatant is obtained, the pH value of the supernatant is adjusted to 1-1.5, and then the first standing is carried out.
In the present invention, the pH of the supernatant is preferably adjusted to 1; the reagent for adjusting the pH value of the supernatant preferably comprises an inorganic acid solution; the inorganic acid solution preferably comprises a hydrochloric acid solution, a carbonic acid solution, an acetic acid solution or a nitric acid solution, and more preferably a hydrochloric acid solution; when the reagents used for adjusting the pH value of the supernatant obtained by the solid-liquid separation are the above reagents, the invention has no special limitation on the proportion of the reagents used for adjusting the pH values of different types, and the reagents can be mixed at any proportion; the concentration of a reagent used for adjusting the pH value of the supernatant obtained by the solid-liquid separation is preferably 5.5-6.5 mol/L, and more preferably 6mol/L; the time for the first standing is preferably 30 to 40min, and more preferably 30 to 35min.
The invention can make the dissolved humate (such as R (COONa) by adjusting the pH value of the supernatant to 1-1.5 4 ) With addition of a mineral acid, e.g. HCl, e.g. R (COONa) 4 +2HCl→R(COOH) 4 +2NaCl, so as to dissolve out humic acid and obtain humic acid substances. In addition, the pH value is adjusted by adding acid for acidification, so that the lignin is removed, and the purity of the hemicellulose is improved.
After the first standing, the supernatant after the first standing is subjected to second solid-liquid separation to respectively obtain filtrate and second solid.
In the present invention, the second solid-liquid separation method is preferably filtration. The filtration method is not particularly limited in the present invention, and a filtration method known in the art may be used. In the embodiment of the invention, the filtering mode is specifically filtering by using filter paper.
After the second solid is obtained, the second solid is subjected to second drying to obtain humic acid.
In the present invention, the temperature of the second drying is preferably 40 to 50 ℃, more preferably 45 to 50 ℃, and the time is preferably 12 to 16 hours, more preferably 12 to 15 hours; the drying mode is preferably drying.
After the filtrate is obtained, the washing solution and the filtrate are mixed, and the pH value of the mixed solution obtained by mixing is adjusted to 5.5-7.5.
In the invention, the pH value of the mixed solution is preferably adjusted to 6.5-7.0; the reagent used for adjusting the pH value of the mixed solution preferably comprises an alkali metal hydroxide solution and/or an alkali metal carbonate solution, and more preferably an alkali metal hydroxide solution; the alkali metal hydroxide solution preferably comprises a potassium hydroxide solution or a sodium hydroxide solution, more preferably a potassium hydroxide solution; the alkali metal carbonate solution preferably comprises a potassium carbonate solution; when the reagents used for adjusting the pH value of the mixed solution are the above-mentioned reagents, the proportion of the reagents used for adjusting the pH values of different types is not particularly limited, and the reagents can be mixed at any proportion; the concentration of the reagent used for adjusting the pH of the mixed solution is preferably 5.5 to 6.5mol/L, and more preferably 6mol/L.
After the pH value of the mixed solution is adjusted, absolute ethyl alcohol is added into the mixed solution, and second standing is carried out.
In the present invention, the volume ratio of the absolute ethanol to the mixed solution is preferably (3 to 8): 1, more preferably (4 to 6): 1; the second standing time is preferably 30 to 40min, and more preferably 35 to 40min.
According to the invention, the absolute ethyl alcohol is added into the mixed solution, so that the hemicellulose dissolved in the mixed solution is precipitated and separated out.
After the second standing, the mixed solution after the second standing is subjected to third solid-liquid separation to obtain a third solid.
In the present invention, the third solid-liquid separation method is preferably filtration. The filtration method is not particularly limited in the present invention, and a filtration method known in the art may be used. In the embodiment of the invention, the filtering mode is specifically filtering by using filter paper.
After the third solid is obtained, the third solid is subjected to third drying to obtain hemicellulose.
In the present invention, the temperature of the third drying is preferably 40 to 50 ℃, more preferably 45 to 50 ℃, and the time is preferably 12 to 16 hours, more preferably 12 to 15 hours; the drying mode is preferably drying.
The flow of the method for covering the rotten product by the alkali heat treatment film and synchronously recovering the multiple active components is shown in figure 1. As shown in figure 1, the membrane covered humified products and the alkali extracting solution are mixed and heated to obtain an alkali heat extracting mixture, and solid and supernatant are obtained through solid-liquid separation; washing the solid and drying to obtain cellulose; regulating the pH value of the supernatant, and performing solid-liquid separation to obtain filtrate and humic acid; and (3) mixing the washing liquid and the filtrate to obtain a mixed liquid, adjusting the pH value of the mixed liquid, adding ethanol, and performing solid-liquid separation to obtain hemicellulose.
The technical solutions in the present invention will be clearly and completely described below with reference to the embodiments of the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Taking livestock and poultry manure (with the water content of 70%) and crop straws (with the water content of 20%) with the mass ratio of 1:1 as raw materials, fermenting for 30D under the covering of a semipermeable membrane prepared by two layers of 600D oxford cloth clamping expanded polytetrafluoroethylene to obtain a membrane covered rotten product, air-drying under natural conditions, removing impurities through manual sorting, crushing into fine particles by a crusher, and sieving with a 60-mesh sieve for later use;
taking 1.00g of film covered humus product (0.25 mm), adding 10.00l0.25wt.% potassium hydroxide solution according to the mass ratio of 1; washing the first solid for 7 times by using deionized water until the pH value of a washing liquid is 7.8, and drying the washed solid for 12h at 50 ℃ to obtain cellulose; adjusting the pH value of the supernatant to 1 with 6mol/L hydrochloric acid solution, standing for 30min, and filtering with filter paper to obtain filtrate and solid on the filter paper; then drying the solid on the filter paper at 50 ℃ for 12h to obtain humic acid; and (2) mixing the filtrate and the washing liquid to obtain a mixed liquid, adjusting the pH value of the mixed liquid to 6.5 by using 6mol/L sodium hydroxide solution, adding absolute ethyl alcohol with the volume being 4 times that of the mixed liquid, standing for 35min, filtering by using filter paper, and drying the solid on the filter paper at 50 ℃ for 12h to obtain hemicellulose, wherein the cellulose recovery rate is 29.32%, the hemicellulose recovery rate is 18.17% and the humic acid recovery rate is 8.92%, and the recovery rate calculation method comprises the steps of respectively measuring the contents of extracted cellulose, hemicellulose and humic acid and respectively dividing the contents by the contents of cellulose, hemicellulose and humic acid in the film covering rotting product directly measured by using a conventional test method.
Example 2
Livestock and poultry manure (with the water content of 70%) and crop straws (with the water content of 20%) in a mass ratio of 1:1 are used as raw materials, and are fermented for 30 days under the covering of a semipermeable membrane prepared by wrapping expanded polytetrafluoroethylene by two layers of 600D oxford fabric, so that a film-covered rotten product is obtained, the film-covered rotten product is air-dried under natural conditions, after impurities are removed through manual sorting, the film-covered rotten product is crushed into fine particles by a crusher, and the fine particles are sieved by a 60-mesh sieve for later use;
taking 1.00g of film covered humus product (0.25 mm), adding 10.00l0.50wt.% potassium hydroxide solution according to the mass ratio of 1; washing the first solid for 8 times by using deionized water until the pH value of a washing liquid is 7.5, and drying the washed solid for 12h at 50 ℃ to obtain cellulose; adjusting the pH value of the supernatant to 1 with 6mol/L hydrochloric acid solution, standing for 30min, and filtering with filter paper to obtain filtrate and solid on the filter paper; then drying the solid on the filter paper at 50 ℃ for 12h to obtain humic acid; and (3) mixing the filtrate and the washing solution to obtain a mixed solution, adjusting the pH value of the mixed solution to 6.0 by using 6mol/L sodium hydroxide solution, adding absolute ethyl alcohol with the volume 6 times that of the mixed solution, standing for 30min, filtering by using filter paper, and drying the solid on the filter paper at 50 ℃ for 12h to obtain hemicellulose, wherein the cellulose recovery rate is 31.56%, the hemicellulose recovery rate is 17.80%, and the humic acid recovery rate is 9.23%.
Example 3
Taking livestock and poultry manure (with the water content of 70%) and crop straws (with the water content of 20%) with the mass ratio of 1:1 as raw materials, fermenting for 30D under the covering of a semipermeable membrane prepared by two layers of 600D oxford cloth clamping expanded polytetrafluoroethylene to obtain a membrane covered rotten product, air-drying under natural conditions, removing impurities through manual sorting, crushing into fine particles by a crusher, and sieving with a 60-mesh sieve for later use;
taking 1.00g of film to cover the humified product (0.25 mm), adding 10.00ml L1.00wt.% potassium hydroxide solution according to the mass ratio of 1; washing the first solid for 6 times by using deionized water until the pH value of a washing liquid is 7.9, and drying the washed solid for 12h at 50 ℃ to obtain cellulose; adjusting the pH value of the supernatant to 1 with 6mol/L hydrochloric acid solution, standing for 30min, and filtering with filter paper to obtain filtrate and solid on the filter paper; then drying the solid on the filter paper at 50 ℃ for 12h to obtain humic acid; and (3) mixing the filtrate and the washing solution to obtain a mixed solution, adjusting the pH value of the mixed solution to 7 by using 6mol/L sodium hydroxide solution, adding absolute ethyl alcohol with the volume 6 times that of the mixed solution, standing for 30min, filtering by using filter paper, and drying the solid on the filter paper at 50 ℃ for 12h to obtain hemicellulose, wherein the cellulose recovery rate is 27.29%, the hemicellulose recovery rate is 17.59%, and the humic acid recovery rate is 8.83%.
Example 4
The difference from example 1 is that 0.25wt.% potassium hydroxide solution was replaced with 0.5wt.% potassium hydroxide solution in example 1, and the remainder was identical to example 1.
Example 5
The difference from example 1 is that 0.25wt.% potassium hydroxide solution was replaced with 0.75wt.% potassium hydroxide solution in example 1, and the remainder was identical to example 1.
Example 6
The difference from example 1 is that 0.25wt.% potassium hydroxide solution in example 1 was replaced with 1wt.% potassium hydroxide solution, and the remainder was identical to example 1.
Example 7
The difference from example 1 is that 0.25wt.% potassium hydroxide solution in example 1 was replaced with 1.25wt.% potassium hydroxide solution, and the remainder was identical to example 1.
Performance testing
The contents of cellulose, hemicellulose and humic acid extracted in examples 1 and 4 to 7 were measured, and the recovery rates of the respective components were calculated by dividing the contents by the contents of cellulose, hemicellulose and humic acid in the film-covered rotten product measured directly by a conventional measurement method, respectively, and the results are shown in fig. 3.
As can be seen from FIG. 3, under the condition of keeping the temperature of the alkaline heat treatment process unchanged, along with the increase of the concentration of the alkaline extractant, cellulose, hemicellulose and humic acid in the film-covered humified products can be better recovered. And with the increase of the concentration of the alkali extracting agent, the recovery rate of humic acid is increased and then reduced, the content of cellulose is monotonically decreased, and the content of hemicellulose is monotonically increased.
Although the present invention has been described in detail with reference to the above embodiments, it is to be understood that the present invention is not limited to the details of the embodiments, and that other embodiments may be devised without departing from the spirit and scope of the present invention.
Claims (10)
1. A method for covering a rotting product by an alkali heat treatment film and synchronously recovering multiple active components is characterized by comprising the following steps:
mixing the film covered decomposed product with an alkali extractant solution, and performing alkali heat treatment to obtain an alkali heat treatment mixture; the mass concentration of the alkali extractant solution is 0.25-1.25%;
carrying out first solid-liquid separation on the alkali heat treatment mixture to respectively obtain a first solid and a supernatant;
washing the first solid until the pH value of the washing liquid is 7.2-8.2, and then carrying out first drying to obtain cellulose;
adjusting the pH value of the supernatant to 1-1.5, sequentially performing first standing and second solid-liquid separation to respectively obtain filtrate and a second solid, and performing second drying on the second solid to obtain humic acid;
and mixing the washing liquid with the filtrate, adjusting the pH value of the mixed liquid obtained by mixing to 5.5-7.5, adding absolute ethyl alcohol, sequentially performing second standing and third solid-liquid separation to obtain a third solid, and performing third drying on the third solid to obtain hemicellulose.
2. The method of claim 1, wherein the alkaline extractant solution comprises an alkali metal hydroxide solution or aqueous ammonia.
3. The method of claim 1 or 2, wherein the film covers a mass ratio of dry weight of humified product to alkaline extractant solution of 1:6-15.
4. The method according to claim 1 or 2, wherein the temperature of the alkali heat treatment is 90 to 95 ℃ and the time is 90 to 120min.
5. The method according to claim 1, wherein the reagent for adjusting the pH of the supernatant comprises an inorganic acid solution.
6. The method according to claim 1, wherein the reagent for adjusting the pH of the mixed solution comprises an alkali metal hydroxide solution and/or an alkali metal carbonate solution.
7. The method according to claim 1, wherein the temperatures of the first drying, the second drying and the third drying are independently 40 to 50 ℃.
8. The method of claim 1, wherein the first solid-liquid separation comprises centrifugation and filtration performed sequentially; the speed of the centrifugation is 4000-8000 rpm, and the time is 5-10 min.
9. The method according to claim 1, characterized in that the particle size of the film covering humified products is 0.18-0.28 mm.
10. The method of claim 1, wherein the first resting and the second resting are independently for 30 to 40min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4459149A (en) * | 1982-09-24 | 1984-07-10 | Moran Edward F | Process for treating humus materials |
| US20040261481A1 (en) * | 2001-12-18 | 2004-12-30 | Alejandro Anaya-Olvera | Method of obtaining a concentrate humic extract from organic and inorganic sources |
| CN104231116A (en) * | 2014-09-03 | 2014-12-24 | 稼禾生物股份有限公司 | Method for preparing hemicellulose, humate and feed additive by utilizing straws |
| CN105440166A (en) * | 2015-12-23 | 2016-03-30 | 中国科学院过程工程研究所 | Method used for extracting hemicellulose with low pigment content |
| CN106283795A (en) * | 2016-11-08 | 2017-01-04 | 福建农林大学 | A kind of method separating hemicellulose and cellulose |
| CN114702711A (en) * | 2022-04-27 | 2022-07-05 | 中国环境科学研究院 | Liquid degradable mulching film produced by using humified products and preparation method and application thereof |
-
2022
- 2022-10-10 CN CN202211234960.5A patent/CN115434175B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4459149A (en) * | 1982-09-24 | 1984-07-10 | Moran Edward F | Process for treating humus materials |
| US20040261481A1 (en) * | 2001-12-18 | 2004-12-30 | Alejandro Anaya-Olvera | Method of obtaining a concentrate humic extract from organic and inorganic sources |
| CN104231116A (en) * | 2014-09-03 | 2014-12-24 | 稼禾生物股份有限公司 | Method for preparing hemicellulose, humate and feed additive by utilizing straws |
| CN105440166A (en) * | 2015-12-23 | 2016-03-30 | 中国科学院过程工程研究所 | Method used for extracting hemicellulose with low pigment content |
| CN106283795A (en) * | 2016-11-08 | 2017-01-04 | 福建农林大学 | A kind of method separating hemicellulose and cellulose |
| CN114702711A (en) * | 2022-04-27 | 2022-07-05 | 中国环境科学研究院 | Liquid degradable mulching film produced by using humified products and preparation method and application thereof |
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