CN112175226A - Method for preparing cellulose sponge by using bean dregs - Google Patents
Method for preparing cellulose sponge by using bean dregs Download PDFInfo
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- CN112175226A CN112175226A CN201910591762.6A CN201910591762A CN112175226A CN 112175226 A CN112175226 A CN 112175226A CN 201910591762 A CN201910591762 A CN 201910591762A CN 112175226 A CN112175226 A CN 112175226A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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Abstract
The invention discloses a method for preparing cellulose sponge by bean dregs, which comprises the following steps: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps: the method comprises the following steps of performing alkaline pre-impurity removal on the bean dregs, performing deep oxidation impurity removal on the bean dregs, performing cellulose fibrillation separation on the bean dregs, and preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps: dissolving and regenerating cellulose in a filamentation manner, regulating and forming a cellulose sponge pore passage, removing free ions of the cellulose sponge, and cooling and drying the cellulose sponge; the bean dregs are selected as the raw materials for preparing the cellulose, thereby avoiding the generation of toxic gases such as hydrogen sulfide, carbon dioxide and the like when polyurethane and polystyrene are used as the raw materials for preparing the cellulose in the traditional process, simultaneously improving the utilization rate of the bean dregs, and avoiding the problems of high cost and difficult large-scale application of cellulose dissolution in the traditional process by carrying out impurity removal operation on the bean dregs through alkaline solvent and oxidation treatment.
Description
Technical Field
The invention belongs to the field of cellulose production, and particularly relates to a method for preparing cellulose sponge by using bean dregs.
Background
The sponge has the advantages of good bulkiness, soft texture, good water absorption and the like, and is widely applied to the fields of cleaning, washing, makeup, medical treatment and the like. At present, sponge products sold in the market are mainly derived from polyurethane and polystyrene in petroleum products, can not only cause harm to human bodies after long-term use, but also cause certain pollution to the environment in the production and waste treatment processes, cellulose is a natural biomass resource with the most abundant reserves in the nature, widely exists in plant resources such as trees, straws, cotton, hemp and bamboo, and has the advantages of being recyclable, degradable, free of pollution, good in biocompatibility and the like. Under natural conditions, the final decomposition products of the cellulose are carbon dioxide and water, so the method has no pollution to the environment and no toxicity or harm to organisms, and is a preferred material for preparing the sponge. The cellulose as a high molecular material has the advantages of strong water absorption, high water absorption speed, good wiping effect, easy air drying, no toxicity and the like, is particularly suitable for daily life, the medical industry and the food industry, and has great market application prospect.
At present, there are two main methods for preparing sponges internationally by using cellulose: firstly, cellulose is converted into cellulose sulfonate through reaction and then hydrolyzed to prepare cellulose, but toxic gases such as sulfur dioxide or hydrogen sulfide and the like can be generated by the process to pollute the atmosphere and water sources; secondly, the cellulose is dissolved and regenerated by a solvent to produce the sponge, but the solvent has higher cost and is difficult to be applied on a large scale.
Disclosure of Invention
The invention aims to provide a method for preparing cellulose sponge by using bean dregs, which aims to solve the problems that toxic gases such as sulfur dioxide or hydrogen sulfide and the like are generated in a preparation process of the cellulose sponge, so that the atmosphere and a water source are polluted, and a cellulose dissolving solvent is high in cost and difficult to apply on a large scale.
The invention is realized in such a way, and provides a method for preparing cellulose sponge by using bean dregs, which is characterized by comprising the following steps: the method comprises the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: the bean dregs are subjected to alkaline pre-impurity removal,
and B: deep oxidation and impurity removal of the bean dregs,
and C: carrying out mercerization separation on the soybean dreg cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: the cellulose extracted in the step S1 is filamentized for low-temperature dissolution and regeneration,
step E: d, performing regulation and control molding treatment on the cellulose sponge pore canal dissolved and regenerated in the step D,
step F: removing free ions from the cellulose sponge regulated and formed in the step E,
step G: and F, cooling and drying the cellulose sponge from which the free ions are removed in the step F.
Preferably, the bean dregs in the step S1 are residual materials after making bean curd, soybean milk, and soybean milk.
Preferably, in the step a, the bean dregs are subjected to alkaline pre-impurity removal through an alkaline pre-impurity removal solvent, wherein the alkaline pre-impurity removal solvent is any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and ammonia water.
Preferably, the concentration of the alkaline pre-impurity removal solvent is 5 wt% -30 wt%, the temperature control range in the alkaline pre-impurity removal process of the bean dregs is 50-90 ℃, and the stirring reaction time in the alkaline impurity removal process of the bean dregs is 1-8 hours.
Preferably, in the step B, the bean dregs are deeply oxidized by an oxidation impurity removal solvent, wherein the oxidation impurity removal solvent is any one of sodium sulfate, potassium persulfate, ammonium persulfate, sodium percarbonate, potassium percarbonate, hydrogen peroxide, sodium peroxide and potassium peroxide.
Preferably, the concentration of the oxidation impurity removal solvent in the step B is 5 wt% -30 wt%, the temperature control range in the deep oxidation impurity removal process of the bean dregs is 50-90 ℃, and the oxidation impurity removal solvent and the bean dregs are stirred to react for 1-8 hours.
Preferably, the cellulose fibrillation separation in the step D is any one of probe ultrasonic treatment, water bath ultrasonic treatment, high-speed shearing treatment and high-pressure homogenization treatment.
Preferably, in the step C, the cellulose sponge is subjected to pore channel regulation and forming treatment by uniformly stirring anhydrous sodium sulfate, absorbent cotton and bean dregs and placing the mixture in a refrigerator for ageing for 2 days.
Preferably, in the step F, the cellulose sponge free-state ions are removed by any one of a lime method, a hydroxide method and a sulfide method, until the sulfate ions in the bean dregs cellulose sponge cannot be detected in warm water washing. Compared with the prior art, the invention has the beneficial effects that: the method selects the residual bean dregs after making bean curd, soybean milk and soybean milk as raw materials to be used as the raw materials for making cellulose, avoids generating toxic gases such as hydrogen sulfide and carbon dioxide and the like when polyurethane and polystyrene are used as the raw materials for making cellulose in the traditional process, improves the utilization rate of the bean dregs, removes impurities from the bean dregs through alkaline solvent and oxidation treatment, dissolves and regenerates the cellulose through sodium hydroxide, urea and deionized water, and avoids the problems that the cellulose dissolution cost is high and the large-scale application is difficult in the traditional process.
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FIG. 1 is a schematic flow chart of the details of the present invention;
FIG. 2 is a schematic flow chart of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1 and 2, the present invention provides a method for preparing cellulose sponge from bean dregs, comprising the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: the bean dregs are subjected to alkaline pre-impurity removal,
and B: deep oxidation and impurity removal of the bean dregs,
and C: carrying out mercerization separation on the soybean dreg cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: the cellulose extracted in the step S1 is filamentized for low-temperature dissolution and regeneration,
step E: d, performing regulation and control molding treatment on the cellulose sponge pore canal dissolved and regenerated in the step D,
step F: removing free ions from the cellulose sponge regulated and formed in the step E,
step G: and F, cooling and drying the cellulose sponge from which the free ions are removed in the step F.
In this embodiment, through carrying out basicity to the bean dregs in advance edulcoration and oxidation edulcoration processing, prevent that cellulose fibrillation from extracting the in-process, produce sulfur dioxide gas and hydrogen sulfide gas and dispel sulfur dioxide gas and sulfide gas in the cellulose sponge through dispelling the processing to cellulose sponge free state ion, prevent that cellulose sponge preparation from finishing, remaining sulfate ion.
Further, the bean dregs in the step S1 are the remaining materials after making bean curd, soybean milk, and soybean milk.
In the embodiment, the residual bean dregs after the bean curd, the bean milk and the soybean milk are made are selected as the raw materials of the bean dreg cellulose sponge, so that the utilization rate of the residual bean dregs after the bean curd, the bean milk and the soybean milk are made is increased, and meanwhile, the cellulose sponge made from the residual bean dregs after the bean curd, the bean milk and the soybean milk is finally decomposed into water and carbon dioxide under natural conditions, so that the environment is not polluted, and the environment is not toxic and harmful to organisms.
Further, in the step A, alkaline pre-impurity removal is carried out on the bean dregs through an alkaline pre-impurity removal solvent, wherein the alkaline pre-impurity removal solvent is any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and ammonia water.
In the embodiment, hydrogen chloride gas, carbon dioxide and sulfur dioxide in the bean dregs are removed by the alkaline pre-impurity removal solvent, and when sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and ammonia water are selected to carry out pre-impurity removal treatment on the bean dregs, no new impurities are brought to the bean dregs.
Further, the concentration of the alkaline pre-impurity removal solvent is 5 wt% -30 wt%, the temperature control range in the alkaline pre-impurity removal process of the bean dregs is 50-90 ℃, and the stirring reaction time in the alkaline impurity removal process of the bean dregs is 1-8 hours.
In the implementation process, the concentration of the alkaline pre-impurity removal solvent is 5-30 wt% to carry out pre-impurity removal treatment on the bean dregs, when the concentration of the alkaline pre-impurity removal solvent is 10-15 wt% to carry out the fastest pre-impurity removal treatment on the bean dregs, the temperature is controlled to be 50-90 ℃ in the alkaline pre-impurity removal process of the bean dregs, the alkaline impurity removal solvent starts to react with the bean dregs, when the temperature is controlled to be 60-80 ℃, the alkaline pre-impurity removal efficiency is fastest, the alkaline pre-impurity removal solvent and the bean dregs are stirred to react for 1-8 hours to accelerate the reaction, and when the alkaline pre-impurity removal solvent is stirred with the bean dregs for 2-3 hours, the alkaline pre-impurity removal solvent thoroughly removes hydrogen chloride gas, carbon dioxide and sulfur dioxide in the bean dregs.
Further, in the step B, deep oxidation treatment is carried out on the bean dregs through an oxidation impurity removal solvent, wherein the oxidation impurity removal solvent is any one of sodium sulfate, potassium persulfate, ammonium persulfate, sodium percarbonate, potassium percarbonate, hydrogen peroxide, sodium peroxide and potassium peroxide.
In the embodiment, water molecules in the bean dregs are removed by the oxidation impurity removal solvent, and the sodium sulfate, the potassium persulfate, the ammonium persulfate, the sodium percarbonate, the potassium percarbonate, the hydrogen peroxide, the sodium peroxide and the potassium peroxide are simultaneously selected, so that new impurities cannot be brought to the bean dregs while the water molecules in the bean dregs are removed.
And further, the concentration of the oxidation impurity removal solvent in the step B is 5 wt% -30 wt%, the temperature control range in the deep oxidation impurity removal process of the bean dregs is 50-90 ℃, and the oxidation impurity removal solvent and the bean dregs are stirred to react for 1-8 hours.
In the embodiment, the concentration of the oxidation impurity removal solvent is 5-30 wt% to remove impurities from the bean dregs, when the concentration of the oxidation impurity removal solvent is 10-15 wt% to remove impurities from the bean dregs in advance, the efficiency of the oxidation impurity removal solvent is fastest, when the temperature is controlled to be 50-90 ℃ in the deep oxidation impurity removal process of the bean dregs, the oxidation impurity removal solvent starts to react with the bean dregs, when the temperature is controlled to be 60-80 ℃, the efficiency of the oxidation impurity removal is fastest, and when the oxidation impurity removal solvent and the bean dregs are stirred to react for 1-8 hours, the reaction is accelerated, and when the oxidation impurity removal solvent and the bean dregs are stirred for 2-3 hours, water molecules in the bean dregs are thoroughly removed by the oxidation impurity removal.
And further, in the step D, the cellulose is subjected to fibrillation separation and is subjected to any one of probe ultrasonic treatment, water bath ultrasonic treatment, high-speed shearing treatment and high-pressure homogenization treatment.
In the present embodiment, any one of probe ultrasonic treatment, water bath ultrasonic treatment, high-speed shearing treatment, and high-pressure homogenization treatment is selected to perform a cellulose separation operation on the bean dregs to obtain cellulose required for manufacturing cellulose sponge.
And further, in the step C, the cellulose sponge is subjected to pore channel regulation and forming treatment by uniformly stirring anhydrous sodium sulfate, absorbent cotton and bean dregs and placing the mixture in a refrigerator for ageing for 2 days.
In the embodiment, the anhydrous sodium sulfate, the absorbent cotton and the bean dregs are uniformly stirred and placed in a refrigerator for being aged for 2 days, the cellulose sponge is subjected to pore channel forming treatment, the anhydrous sodium sulfate is stable and insoluble in strong acid, aluminum and magnesium, and the absorbent cotton increases the strength of the bean dregs cellulose sponge.
And further, in the step F, removing free ions from the cellulose sponge by any one of a lime method, a hydroxide method and a sulfide method until sulfate ions in the bean dregs cellulose sponge cannot be detected in warm water washing. In the present embodiment, the heavy metal ions and the inorganic salt ions in the cellulose sponge are removed by any of the lime method, the hydroxide method, and the sulfide method.
In the embodiment, bean curd making bean dregs are selected as raw materials for cellulose extraction, alkaline pre-impurity removal is carried out on the bean dregs through an alkaline impurity removal solvent, hydrogen chloride gas, carbon dioxide and sulfur dioxide in the bean dregs are removed, water molecules in the bean dregs are removed through an oxidation impurity removal agent, finally, cellulose is separated in a fibrillation mode to the bean dregs to obtain cellulose, the cellulose is dissolved and regenerated, pore regulation and forming processing is carried out on cellulose sponge through anhydrous sodium sulfate, free ions are removed from the cellulose sponge, heavy metal ions in the cellulose sponge are removed, and the cellulose sponge is obtained through cooling and drying.
Example 2
Referring to fig. 1 and 2, the present invention provides a method for preparing cellulose sponge from bean dregs, comprising the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: adding 10.0 wt% of sodium hydroxide to carry out alkaline pre-impurity removal treatment on 100g of bean dregs,
and B: adding 12.5 wt% of sodium percarbonate to carry out deep oxidation impurity removal treatment on 100g of bean dregs,
and C: adding 100ml of deionized water, and carrying out ultrasonic treatment for 30 minutes by using a probe to carry out cellulose fibrillation separation treatment on 100g of bean dregs to obtain 2g of bean dregs cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: 2g of the cellulose extracted in the step S1 is dissolved and regenerated by 3.5g of sodium hydroxide, 6.0g of urea and 38.5g of deionized water at low temperature,
step E: adding 50.5g of anhydrous sodium sulfate to regulate and control the pore canal of the regenerated cellulose 2g of sponge,
step F: washing with deionized water until no sulfate ion can be detected, removing free ions from cellulose 2g,
step G: and F, freezing and drying the free ions in the step F to obtain the cellulose sponge.
In the embodiment, 10.0 wt% of sodium hydroxide, 12.5 wt% of sodium percarbonate and 100mL of deionized water are mixed with 100g of bean dregs, the stirring temperature is controlled to be 60 ℃, the temperature is increased to 90 ℃ after the stirring reaction is carried out for 1 hour, the stirring reaction is carried out for 3 hours, the temperature is reduced after the reaction is finished, the washing is carried out, 200-250 mL of deionized water is added, the stirring and the uniform dispersion are carried out, and the probe ultrasound is carried out for 30min to prepare 2g of bean dregs cellulose.
In the embodiment, 2g of bean dregs cellulose, 3.5g of sodium hydroxide, 6.0g of urea and 38.5g of deionized water are mixed, the mixture is stirred uniformly by magnetic force, the mixture is placed in a refrigerator to be frozen overnight, the cellulose is dissolved and regenerated, the mixture is unfrozen at room temperature, 0.5g of absorbent cotton with the length less than 2mm is added under the stirring by magnetic force, the mixture is stirred uniformly, 50.5g of anhydrous sodium sulfate is added, a pore passage is adjusted, the mixture is placed in the refrigerator to be aged for 2 days, the mixture is unfrozen at room temperature, the mixture is washed by deionized water until sulfate ions cannot be detected, and the cellulose sponge.
Example 3
Referring to fig. 1 and 2, the present invention provides a method for preparing cellulose sponge from bean dregs, comprising the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: adding potassium hydroxide 15.0 wt% to carry out alkaline pre-impurity removal treatment on 100g of bean dregs,
and B: adding potassium percarbonate 15.0 wt% to carry out deep oxidation impurity removal treatment on 100g of bean dregs,
and C: adding 100ml of deionized water, and carrying out cellulose fibrillation separation treatment on 100g of bean dregs by water bath ultrasound for 60 minutes to obtain 2g of bean dregs cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: dissolving and regenerating 2g of cellulose extracted in the step S1 by 3.5g of sodium hydroxide, 6.0g of urea and 40.0g of deionized water at low temperature,
step E: adding 40.0g of anhydrous sodium sulfate to regulate and control the pore canal of the sponge containing 2g of dissolved and regenerated cellulose,
step F: washing with deionized water until no sulfate ion can be detected, removing free ions from cellulose 2g,
step G: and F, freezing and drying the free ions in the step F to obtain the cellulose sponge.
In the embodiment, 15.0 wt% of potassium hydroxide, 15.0 wt% of potassium percarbonate and 100mL of deionized water are mixed with 100g of bean dregs, the stirring temperature is controlled to be 50 ℃, the temperature is increased to 80 ℃ after the stirring reaction is carried out for 1 hour, the stirring reaction is carried out for 3 hours, the temperature is reduced after the reaction is finished, the washing is carried out, 200-250 mL of deionized water is added, the stirring and the uniform dispersion are carried out, and the water bath ultrasound is carried out for 30min, so that 2g of bean dregs cellulose is prepared.
In the embodiment, 2g of bean dregs cellulose, 3.5g of sodium hydroxide, 6.0g of urea and 40.0g of deionized water are mixed, the mixture is stirred uniformly by magnetic force, the mixture is placed in a refrigerator to be frozen overnight, the cellulose is dissolved and regenerated, the mixture is unfrozen at room temperature, 0.5g of absorbent cotton with the length less than 1mm is added under the stirring by magnetic force, the mixture is stirred uniformly, 40g of anhydrous sodium sulfate is added, a pore passage is adjusted, the mixture is placed in the refrigerator to be aged for 2 days, the mixture is unfrozen at room temperature, the mixture is washed by deionized water until no sulfate ion is detected, and the cellulose sponge.
Example 4
Referring to fig. 1 and 2, the present invention provides a method for preparing cellulose sponge from bean dregs, comprising the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: adding 10.0 wt% of ammonia water to carry out alkaline pre-impurity removal treatment on 100g of bean dregs,
and B: adding 10.0 wt% of ammonium persulfate to carry out deep oxidation impurity removal treatment on 100g of bean dregs,
and C: adding 100ml of deionized water, and performing cellulose fibrillation separation treatment on 100g of bean dregs by high-speed shearing for 20 minutes to obtain 2g of bean dregs cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: dissolving and regenerating 2g of cellulose extracted in the step S1 by 3.5g of sodium hydroxide, 6.0g of urea and 30.0g of deionized water at low temperature,
step E: 35.0g of anhydrous sodium sulfate is added to regulate and control the forming treatment of 2g of sponge pore canals of the dissolved and regenerated cellulose,
step F: washing with deionized water until no sulfate ion can be detected, removing free ions from cellulose 2g,
step G: and F, freezing and drying the free ions in the step F to obtain the cellulose sponge.
In the embodiment, 10.0 wt% of ammonia water, 10.0 wt% of ammonium persulfate and 100mL of deionized water are mixed with 100g of bean dregs, the stirring temperature is controlled to be 50 ℃, after the stirring reaction is carried out for 1 hour, the temperature is raised to 90 ℃, the stirring reaction is carried out for 2 hours, after the reaction is finished, the temperature is reduced, the washing is carried out, 200-250 mL of deionized water is added, after the uniform stirring and dispersion, the water bath ultrasound is carried out for 30min, and 2g of bean dregs cellulose is prepared.
In the embodiment, 2g of bean dregs cellulose, 3.5g of sodium hydroxide, 6.0g of urea and 40.0g of deionized water are mixed, the mixture is stirred uniformly by magnetic force, the mixture is placed in a refrigerator to be frozen overnight, the cellulose is dissolved and regenerated, the mixture is unfrozen at room temperature, 0.5g of absorbent cotton with the length of less than 3mm is added under the stirring by magnetic force, the mixture is stirred uniformly, 35.0g of anhydrous sodium sulfate is added, a pore passage is adjusted, the mixture is placed in the refrigerator to be aged for 2 days, the mixture is unfrozen at room temperature, the deionized water is washed until sulfate ions are not detected, and the cellulose sponge is.
Example 5
Referring to fig. 1 and 2, the present invention provides a method for preparing cellulose sponge from bean dregs, comprising the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: adding 10.0 wt% of sodium hydroxide to carry out alkaline pre-impurity removal treatment on 100g of bean dregs,
and B: adding 10.0 wt% of hydrogen peroxide to carry out deep oxidation impurity removal treatment on 100g of bean dregs,
and C: adding 100ml of deionized water, and performing cellulose fibrillation separation treatment on 100g of bean dregs by high-speed shearing for 20 minutes to obtain 2g of bean dregs cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: dissolving and regenerating 2g of cellulose extracted in the step S1 by 4.0g of sodium hydroxide, 6.0g of urea and 35.0g of deionized water at low temperature,
step E: adding 55.0g of anhydrous sodium sulfate to regulate and control the pore canal of the regenerated cellulose 2g of sponge,
step F: washing with deionized water until no sulfate ion can be detected, removing free ions from cellulose 2g,
step G: and F, freezing and drying the free ions in the step F to obtain the cellulose sponge.
In the embodiment, 10.0 wt% of sodium hydroxide, 10.0 wt% of hydrogen peroxide and 30.0g of deionized water are mixed with 100g of bean dregs, the stirring temperature is controlled to be 50 ℃, after stirring and reacting for 1 hour, the temperature is increased to 80 ℃, stirring and reacting for 2 hours, after the reaction is finished, the temperature is reduced, washing is carried out, 200-250 mL of deionized water is added, after stirring and dispersing uniformly, high-pressure homogenization is carried out for 5 times, and 2g of bean dregs cellulose is prepared.
In the embodiment, 2g of bean dregs cellulose, 4.0g of sodium hydroxide, 6.0g of urea and 35.0g of deionized water are mixed, the mixture is stirred uniformly by magnetic force, the mixture is placed in a refrigerator to be frozen overnight, the cellulose is dissolved and regenerated, the mixture is unfrozen at room temperature, 0.5g of absorbent cotton with the length less than 0.5mm is added under the stirring by magnetic force, the mixture is stirred uniformly, 55.0g of anhydrous sodium sulfate is added, a pore channel is adjusted, the mixture is placed in the refrigerator to be aged for 2 days, the mixture is unfrozen at room temperature, the mixture is washed by deionized water until sulfate ions are not detected, and the cellulose sponge.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A method for preparing cellulose sponge by using bean dregs is characterized by comprising the following steps: the method comprises the following steps:
step S1: extracting the cellulose of the bean dregs, wherein the extraction of the cellulose of the bean dregs comprises the following steps:
step A: the bean dregs are subjected to alkaline pre-impurity removal,
and B: deep oxidation and impurity removal of the bean dregs,
and C: carrying out mercerization separation on the soybean dreg cellulose;
step S2: preparing the bean dreg cellulose sponge, wherein the preparation of the bean dreg cellulose sponge comprises the following steps:
step D: the cellulose extracted in the step S1 is filamentized for low-temperature dissolution and regeneration,
step E: d, performing regulation and control molding treatment on the cellulose sponge pore canal dissolved and regenerated in the step D,
step F: removing free ions from the cellulose sponge regulated and formed in the step E,
step G: and F, cooling and drying the cellulose sponge from which the free ions are removed in the step F.
2. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 1, which is characterized in that: the bean dregs in the step S1 are the remaining materials after making bean curd, soybean milk, and soybean milk.
3. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 1, which is characterized in that: and B, performing alkaline pre-impurity removal on the bean dregs by using an alkaline pre-impurity removal solvent in the step A, wherein the alkaline pre-impurity removal solvent is any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and ammonia water.
4. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 3, which is characterized in that: the concentration of the alkaline pre-impurity removal solvent is 5 wt% -30 wt%, the temperature control range in the bean dreg alkaline pre-impurity removal process is 50-90 ℃, and the stirring reaction time in the bean dreg alkaline impurity removal process is 1-8 hours.
5. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 1, which is characterized in that: and in the step B, deep oxidation treatment is carried out on the bean dregs through an oxidation impurity removal solvent, wherein the oxidation impurity removal solvent is any one of sodium sulfate, potassium persulfate, ammonium persulfate, sodium percarbonate, potassium percarbonate, hydrogen peroxide, sodium peroxide and potassium peroxide.
6. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 5, wherein the method comprises the following steps: and B, the concentration of the oxidation impurity removal solvent in the step B is 5-30 wt%, the temperature control range in the deep oxidation impurity removal process of the bean dregs is 50-90 ℃, and the oxidation impurity removal solvent and the bean dregs are stirred to react for 1-8 hours.
7. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 1, which is characterized in that: and D, performing cellulose fibrillation separation to obtain any one of probe ultrasonic treatment, water bath ultrasonic treatment, high-speed shearing treatment and high-pressure homogenization treatment.
8. The method for preparing the cellulose sponge from the bean dregs as claimed in claim 1, wherein in the step C, the cellulose sponge is subjected to pore channel regulation and forming treatment by uniformly stirring the anhydrous sodium sulfate, the absorbent cotton and the bean dregs and placing the mixture in a refrigerator for ageing for 2 days.
9. The method for preparing the cellulose sponge by using the bean dregs as claimed in claim 1, which is characterized in that: and F, removing free ions of the cellulose sponge by adopting any one of a lime method, a hydroxide method and a sulfide method until sulfate ions in the bean dregs cellulose sponge cannot be detected in warm water washing.
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| CN201910591762.6A CN112175226A (en) | 2019-07-01 | 2019-07-01 | Method for preparing cellulose sponge by using bean dregs |
| PCT/CN2019/127487 WO2021000542A1 (en) | 2019-07-01 | 2019-12-23 | Method for preparing cellulose sponge using bean dregs |
| JP2021535095A JP7165825B2 (en) | 2019-07-01 | 2019-12-23 | Method for preparing cellulose sponge using okara |
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| CN102634069A (en) * | 2012-04-25 | 2012-08-15 | 桂林理工大学 | Method for preparing hemostatic sponge by use of sisal cellulose oxide |
| US20170182203A1 (en) * | 2015-12-28 | 2017-06-29 | Hangzhou Singclean Medical Products Co., Ltd | Method for preparing oxidized cellulose hemostatic product |
| CN107232613A (en) * | 2017-07-04 | 2017-10-10 | 华南理工大学 | A kind of method of ultrasonic wave added thermokalite method combined extracting soybean fiber and bean dregs albumen |
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| JP3213648B2 (en) * | 1993-03-03 | 2001-10-02 | 日本たばこ産業株式会社 | Method for producing water-soluble polysaccharide |
| AT402932B (en) * | 1995-12-22 | 1997-09-25 | Chemiefaser Lenzing Ag | CELLULOSE SPONGE AND METHOD FOR THE PRODUCTION THEREOF |
| JP2001172302A (en) * | 1999-12-16 | 2001-06-26 | Rengo Co Ltd | Cellulose carbamate sponge and its production method |
| JP4054968B2 (en) * | 2002-04-24 | 2008-03-05 | 信越化学工業株式会社 | Method for producing low-substituted cellulose ether sponge body |
| CN100998381B (en) * | 2006-12-12 | 2010-12-01 | 南昌大学 | Method for producing high purity nanometer grain dietary fiber |
| JP4905814B2 (en) * | 2009-10-09 | 2012-03-28 | 国立大学法人 東京大学 | Composite porous material and method for producing the same |
| CN103741532B (en) * | 2013-12-23 | 2015-11-25 | 江南大学 | A kind of can the preparation method of nano-cellulose fiber of strong adsorption grease and cholate |
| WO2017141910A1 (en) * | 2016-02-15 | 2017-08-24 | 東ソー株式会社 | Porous crosslinked cellulose gel and manufacturing method for same |
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| CN107417980B (en) * | 2017-06-23 | 2019-05-17 | 天长市博资清洁科技有限公司 | The preparation method of wood pulp sponge |
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| CN102634069A (en) * | 2012-04-25 | 2012-08-15 | 桂林理工大学 | Method for preparing hemostatic sponge by use of sisal cellulose oxide |
| US20170182203A1 (en) * | 2015-12-28 | 2017-06-29 | Hangzhou Singclean Medical Products Co., Ltd | Method for preparing oxidized cellulose hemostatic product |
| CN107232613A (en) * | 2017-07-04 | 2017-10-10 | 华南理工大学 | A kind of method of ultrasonic wave added thermokalite method combined extracting soybean fiber and bean dregs albumen |
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| WO2021000542A1 (en) | 2021-01-07 |
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