CN106905411B - Method for preparing white mustard seed protein powder and using white mustard seed protein powder to treat anionic dye wastewater - Google Patents

Method for preparing white mustard seed protein powder and using white mustard seed protein powder to treat anionic dye wastewater Download PDF

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Publication number
CN106905411B
CN106905411B CN201710066665.6A CN201710066665A CN106905411B CN 106905411 B CN106905411 B CN 106905411B CN 201710066665 A CN201710066665 A CN 201710066665A CN 106905411 B CN106905411 B CN 106905411B
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white mustard
mustard seed
powder
stirring
protein powder
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CN106905411A (en
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帖靖玺
牛亚芬
常淦钫
常阳阳
石玲
余璐
姬一凡
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North China University of Water Resources and Electric Power
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/36Extraction; Separation; Purification by a combination of two or more processes of different types
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/30Extraction; Separation; Purification by precipitation
    • C07K1/303Extraction; Separation; Purification by precipitation by salting out
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/30Extraction; Separation; Purification by precipitation
    • C07K1/306Extraction; Separation; Purification by precipitation by crystallization
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/34Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

Abstract

The method for preparing the white mustard seed protein powder and using the white mustard seed protein powder to treat anionic dye wastewater comprises the following steps: pulverizing semen Sinapis Albae into powder; mixing the white mustard seed powder and the ammonium sulfate solution, and extracting protein by low-temperature ultrasound or stirring at room temperature; filtering the mixed solution; carrying out protein extraction on filter residues for multiple times; mixing the filtrates, continuously adding ammonium sulfate powder, and stirring; carrying out centrifugal treatment on the mixed solution; collecting the precipitate and dialyzing; putting the dialyzate into an open flat-bottomed container for low-temperature vacuum drying; the dried light yellow crystal is the dry powder of the white mustard seed protein; preparing the protein powder into active protein liquid, adding the active protein liquid into the anionic dye wastewater to be treated, stirring and precipitating to remove the anionic dye in the water. The invention has the advantages of simple and convenient preparation of the active protein powder of white mustard seed, simple equipment, simple and convenient operation and the like, and the prepared active protein powder of white mustard seed provides a new method for removing certain types of anionic dyes in water.

Description

Method for preparing white mustard seed protein powder and using white mustard seed protein powder to treat anionic dye wastewater
Technical Field
The invention belongs to the technical field of environment-friendly water treatment, and particularly relates to a method for preparing white mustard seed protein powder and a method for treating anionic dye wastewater by using the white mustard seed protein powder.
Background
China is a large textile production country and, according to statistics,the production of its textile fibers was 2/3 worldwide in 2012. In order to meet the requirement of textile production, China needs to produce a large amount of dyes every year, and at present, China is the first dye producing country in the world. The annual yield of commercial dye in 2013 nationwide is 8.95 multiplied by 10 according to statistics5Ton, 65% of the annual production worldwide.
In the using process, about 30% of dye is discharged along with the wastewater, and the discharge amount of the printing and dyeing wastewater accounts for 17% -20% of the discharge amount of the industrial wastewater in the world according to the statistics of the world bank. In 2013, the discharge amount of Chinese dye wastewater reaches 1.96 multiplied by 109Cubic meter. The printing and dyeing wastewater has the characteristics of complex components, high pollutant content, high chromaticity, high toxicity and the like, so the dye wastewater can be discharged after standard treatment.
The currently common dye wastewater treatment methods mainly comprise: biological method, advanced oxidation method, adsorption method, reverse osmosis method, coagulation method, etc. Among them, the biological method and coagulation method are methods convenient for large-scale popularization, but because synthetic dyes contain aromatic ring structures, the synthetic dyes have high biological stability, the conventional biological treatment effect is poor, and some dyes or decomposed intermediates thereof have three properties, so the conventional biological treatment is not an ideal treatment mode of dye wastewater. The coagulation method has the characteristics of strong adaptability, simple operation and management, low capital investment, mature technology and the like. Therefore, the coagulation method is a dye wastewater treatment method which is widely applied industrially.
The coagulant is the key to ensure that the coagulation method obtains good treatment effect. The current commercial coagulants are mainly iron salt or aluminum salt coagulants. However, most of the raw materials of the coagulant used for wastewater treatment are industrial wastes, and the coagulant itself contains heavy metal ions, which are left to easily cause secondary pollution, and the remaining aluminum ions are harmful to human bodies. Therefore, it is very urgent and necessary to find a natural coagulant which is safe to human and environment and is non-toxic.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a safe, non-toxic, environment-friendly and energy-saving method for preparing white mustard seed protein powder and a method for treating anionic dye wastewater by using the white mustard seed protein powder.
In order to solve the technical problems, the invention adopts the following technical scheme: the method for preparing the white mustard seed protein powder and using the white mustard seed protein powder to treat the anionic dye wastewater comprises the following steps,
(1) drying semen Sinapis Albae at low temperature for 1-3 hr, pulverizing, sieving, and making into semen Sinapis Albae powder;
(2) mixing the white mustard seed powder with an ammonium sulfate solution, and then extracting water-soluble protein in the white mustard seeds under the conditions of low-temperature ultrasound or normal-temperature stirring;
(3) taking out the mixed liquid treated in the step (2), filtering by using a 0.22 micron filter membrane, and respectively collecting filtrate and filter residue;
(4) repeatedly extracting the filter residue according to the method shown in the steps (2) and (3);
(5) discarding filter residues after multiple extractions, mixing the collected filtrates, slowly adding ammonium sulfate powder to a certain saturation while stirring, and continuously stirring at room temperature for 30 minutes;
(6) centrifuging the mixed solution obtained in the step (5), and collecting precipitates;
(7) putting the precipitate obtained in the step (6) into a dialysis bag, sealing the dialysis bag, and desalting the dialysis bag in deionized water;
(8) taking the desalted dialysate obtained in the step (7) out of the dialysis bag, and pouring the dialysate into a flat-bottom open container;
(9) putting the container into an electric heating vacuum drying oven for low-temperature vacuum drying until the water is completely evaporated, and separating out light yellow needle-shaped crystal which is the active protein powder of the white mustard seed;
(10) and (3) adding a certain amount of protein liquid prepared from the protein powder in the step (9) into the anionic dye wastewater to be treated, firstly stirring at a slow speed, then stirring at a fast speed and precipitating for a period of time, thus removing the anionic dye in the wastewater.
In the step (1), the white mustard seeds need to be crushed and sieved, and the particle size is smaller than 80 meshes.
The concentration of the ammonium sulfate solution in the step (2) is 0.2-1.0 mol/L, and the mixing ratio of the white mustard seed powder and the ammonium sulfate is the weight of the white mustard seed powder: ammonium sulfate solution volume =1:10-1:30, mustard powder weight in g, ammonium sulfate solution volume in ml;
the mixed solution in the step (2) is placed in an ice-water mixture for ultrasonic treatment for 3-5 minutes; or stirring the mixture on a magnetic stirrer with 3000 and 4000 revolutions per minute for 5 to 20 minutes; to promote the complete dissolution of the water-soluble protein contained in the white mustard seed powder.
The repeated extraction times in the step (4) are 3-5 times, so that the soluble protein in the white mustard seeds is extracted to the maximum extent, and the raw materials are fully utilized.
The saturation degree of the ammonium sulfate in the step (5) is 80%, the stirring speed is 3000-4000 r/min, and the duration is 30 min.
The rotation speed of the centrifuge in the step (6) is 3000-4000 rpm, and the duration is 10 minutes.
And (3) the cut-off molecular weight of the dialysis bag selected in the step (7) is 6000Da, the sealed dialysis bag filled with the protein liquid is placed in a container filled with deionized water, and water is changed periodically to promote the dissolution of the residual ammonium sulfate in the dialysis bag.
The container used in the step (8) is a flat-bottom, open glass or stainless steel container.
The temperature of the electric heating vacuum drying oven in the step (9) is 40 ℃, and the vacuum degree is 0.06-0.08 MPa;
and (3) in the step (10), slowly stirring for 30 seconds to 1 minute, quickly stirring for 15 to 30 minutes, and precipitating for 1 to 3 hours.
By adopting the technical scheme, the raw material of the invention is cheap and easily available white mustard seed, and the way of using the extract of the white mustard seed in water treatment opens up a new way for the utilization of the white mustard seed. The method has the advantages of simple preparation, simple equipment, simple and convenient operation, safety, environmental protection and the like of the active white mustard seed protein powder, and the prepared active white mustard seed protein powder provides a new method for removing certain types of anionic dyes in water. The method has the advantages of simple process, strong practicability, good removal effect on certain anionic dyes (such as direct suntan G, reactive green 19, direct yellow R and the like) in water, and easy popularization and application.
Detailed Description
The method for preparing the white mustard seed protein powder and using the white mustard seed protein powder to treat the anionic dye wastewater comprises the following steps,
(1) drying semen Sinapis Albae at low temperature for 1-3 hr, pulverizing, sieving, and making into semen Sinapis Albae powder;
(2) mixing the white mustard seed powder with an ammonium sulfate solution, and then extracting water-soluble protein in the white mustard seeds under the conditions of low-temperature ultrasound or normal-temperature stirring;
(3) taking out the mixed liquid treated in the step (2), filtering by using a 0.22 micron filter membrane, and respectively collecting filtrate and filter residue;
(4) repeatedly extracting the filter residue according to the method shown in the steps (2) and (3);
(5) discarding filter residues after multiple extractions, mixing the filtrates collected each time, slowly adding ammonium sulfate powder to a certain saturation degree while stirring, and continuously stirring for 30 minutes at room temperature;
(6) centrifuging the mixed solution obtained in the step (5), and collecting precipitates;
(7) putting the precipitate obtained in the step (6) into a dialysis bag, sealing the dialysis bag, and desalting the dialysis bag in deionized water;
(8) taking the desalted dialysate obtained in the step (7) out of the dialysis bag, and pouring the dialysate into a flat-bottom open container;
(9) putting the container into an electric heating vacuum drying oven for low-temperature vacuum drying until the water is completely evaporated, and separating out light yellow needle-shaped crystal which is the active protein powder of the white mustard seed;
(10) and (3) adding a certain amount of protein liquid prepared from the protein powder in the step (9) into the anionic dye wastewater to be treated, firstly stirring at a slow speed, then stirring at a fast speed and precipitating for a period of time, thus removing the anionic dye in the wastewater.
In the step (1), the white mustard seeds need to be crushed and sieved, and the particle size is smaller than 80 meshes.
The concentration of the ammonium sulfate solution in the step (2) is 0.2-1.0 mol/L, and the mixing ratio of the white mustard seed powder and the ammonium sulfate is the weight of the white mustard seed powder: ammonium sulfate solution volume =1:10-1:30, mustard powder weight in g, ammonium sulfate solution volume in ml;
the mixed solution in the step (2) is placed in an ice-water mixture for ultrasonic treatment for 3-5 minutes; or stirring the mixture on a magnetic stirrer with 3000 and 4000 revolutions per minute for 5 to 20 minutes; to promote the complete dissolution of the water-soluble protein contained in the white mustard seed powder.
The repeated extraction times in the step (4) are 3-5 times, so that the soluble protein in the white mustard seeds is extracted to the maximum extent, and the raw materials are fully utilized.
The saturation degree of the ammonium sulfate in the step (5) is 80%, the stirring speed is 3000-4000 r/min, and the duration time is 30 min.
The rotation speed of the centrifuge in the step (6) is 3000-4000 rpm, and the duration is 10 minutes.
And (3) the cut-off molecular weight of the dialysis bag selected in the step (7) is 6000Da, the sealed dialysis bag filled with the protein liquid is placed in a container filled with deionized water, and water is changed periodically to promote the dissolution of the residual ammonium sulfate in the dialysis bag.
The container used in the step (8) is a flat-bottom, open glass or stainless steel container.
The temperature of the electric heating vacuum drying oven in the step (9) is 40 ℃, and the vacuum degree is 0.06-0.08 MPa.
And (3) in the step (10), slowly stirring for 30 seconds to 1 minute, quickly stirring for 15 to 30 minutes, and precipitating for 1 to 3 hours.
The invention is further described below with reference to specific examples:
(1) mixing 1 g of the white mustard seed powder which is sieved by a 80-mesh sieve with 1 mol/L of ammonium sulfate solution according to the mass of the white mustard seed powder: mixing ammonium sulfate solution according to the volume =1:20 ratio, and then stirring for 20 minutes on a magnetic stirrer at the rotating speed of 4000 revolutions per minute;
(2) filtering the stirred mixed solution by adopting a 0.22 micron filter membrane, and collecting the filtrate;
(3) adding ammonium sulfate powder into the filtrate until the filtrate is saturated by 80%, and continuing stirring for about 30 minutes after the addition is finished;
(4) repeatedly extracting the filter residue according to the method shown in the steps (2) and (3);
(5) centrifuging the mixed solution in a centrifugal machine with the speed of 4000 revolutions per minute for 10 minutes, and collecting precipitates;
(6) adding the precipitate into a dialysis bag with the molecular weight cutoff of 6000Da, sealing two ends of the dialysis bag, putting the dialysis bag into a container filled with distilled water, and periodically changing water until no precipitate appears when barium sulfate is added into the water in the container, thus completing desalination;
(7) taking out the desalted dialysate from the permeable bag and putting the dialysate into a flat-bottom stainless steel tray;
(8) putting the tray into an electric heating vacuum drying oven with the temperature of 40 ℃ and the vacuum degree of 0.06 MPa until the water is evaporated to dryness, and separating out light yellow crystals, namely the white mustard seed protein powder;
(9) taking a certain amount of the protein powder, and preparing 5 g/L protein liquid by using distilled water;
(10) 200 ml of simulated dye wastewater prepared by using tap water and direct suntan G is put on a six-connection stirrer, firstly the wastewater is rapidly stirred for 1 minute at the speed of 120 revolutions per minute, then the wastewater is slowly stirred for 20 minutes at the speed of 45 revolutions per minute, and then the wastewater is statically settled for 2 hours, so that the anionic dye can be removed from the water. The experimental results are shown in table one;
table-test parameter table
Figure DEST_PATH_IMAGE001
The present embodiment is not intended to limit the materials, processes, etc. of the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are all within the scope of the technical solution of the present invention.

Claims (8)

1. The method for treating anionic dye wastewater by using the white mustard seed protein powder is characterized by comprising the following steps of: comprises the following steps of (a) carrying out,
(1) drying semen Sinapis Albae at low temperature for 1-3 hr, pulverizing, sieving, and making into semen Sinapis Albae powder;
(2) mixing the white mustard seed powder with an ammonium sulfate solution, and then extracting water-soluble protein in the white mustard seed powder under the condition of stirring at normal temperature;
(3) taking out the mixed liquid treated in the step (2), filtering by using a 0.22 micron filter membrane, and respectively collecting filtrate and filter residue;
(4) repeatedly extracting the filter residue according to the method shown in the steps (2) and (3);
(5) discarding filter residues after multiple extractions, mixing the filtrates collected each time, slowly adding ammonium sulfate powder to reach 80% saturation while stirring, and continuously stirring at room temperature for 30 minutes;
(6) centrifuging the mixed solution obtained in the step (5), and collecting precipitates;
(7) putting the precipitate in the step (6) into a dialysis bag, sealing the dialysis bag and desalting in deionized water;
(8) taking the desalted dialysate obtained in the step (7) out of the dialysis bag, and pouring the dialysate into a flat-bottom open container;
(9) putting the container into an electric heating vacuum drying oven for low-temperature vacuum drying until the water is completely evaporated, and separating out a light yellow crystal which is the active protein powder of the white mustard seed;
(10) adding a certain amount of protein liquid prepared from the protein powder in the step (9) into the to-be-treated anionic dye wastewater containing direct suntan G, firstly stirring at a slow speed, then stirring at a fast speed and precipitating for a period of time, and then removing the anionic dye in the wastewater;
in the step (1), the white mustard seeds need to be crushed and sieved, and the particle size is smaller than 80 meshes;
the concentration of the ammonium sulfate solution in the step (2) is 0.2-1.0 mol/L, and the mixing ratio of the white mustard seed powder and the ammonium sulfate is the weight of the white mustard seed powder: ammonium sulfate solution volume =1:10-1:30, mustard powder weight in g, ammonium sulfate solution volume in ml;
the mixed solution in the step (2) is placed on a magnetic stirrer with 3000-4000 rpm for stirring for 5-20 minutes; to promote the complete dissolution of the water-soluble protein contained in the white mustard seed powder.
2. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1, wherein the method comprises the following steps: the repeated extraction times in the step (4) are 3-5 times, so that the soluble protein in the white mustard seeds is extracted to the maximum extent, and the raw materials are fully utilized.
3. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1, wherein the method comprises the following steps: the stirring speed in the step (5) is 3000-4000 rpm, and the duration is 30 minutes.
4. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1, wherein the method comprises the following steps: the rotation speed of the centrifugation in the step (6) is 3000-4000 rpm, and the duration time is 10 minutes.
5. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1 or 2, which is characterized in that: and (3) the cut-off molecular weight of the dialysis bag selected in the step (7) is 6000Da, the sealed dialysis bag filled with the protein liquid is placed in a container filled with deionized water, and water is changed periodically to promote the dissolution of the residual ammonium sulfate in the dialysis bag.
6. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1 or 2, which is characterized in that: the container used in the step (8) is a flat-bottom, open glass or stainless steel container.
7. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1 or 2, which is characterized in that: the temperature of the electric heating vacuum drying oven in the step (9) is 40 ℃, and the vacuum degree is 0.06-0.08 MPa.
8. The method for treating anionic dye wastewater by using the white mustard seed protein powder as claimed in claim 1 or 2, which is characterized in that: and (3) in the step (10), slowly stirring for 30 seconds to 1 minute, quickly stirring for 15 to 30 minutes, and precipitating for 1 to 3 hours.
CN201710066665.6A 2017-02-07 2017-02-07 Method for preparing white mustard seed protein powder and using white mustard seed protein powder to treat anionic dye wastewater Expired - Fee Related CN106905411B (en)

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