CN111153475A - Flocculating agent for stevioside extraction - Google Patents
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- CN111153475A CN111153475A CN201910914477.3A CN201910914477A CN111153475A CN 111153475 A CN111153475 A CN 111153475A CN 201910914477 A CN201910914477 A CN 201910914477A CN 111153475 A CN111153475 A CN 111153475A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
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Abstract
A flocculating agent for stevioside extraction comprises the following raw materials in parts by weight: 5-9 parts of chitosan, 15-25 parts of lignin, 10-18 parts of ammonium persulfate, 20-25 parts of polyaluminum ferric sulfate, 22-24 parts of aluminum citrate, 2-7 parts of magnesium sulfate, 1-4 parts of calcium chloride, 15-25 parts of polysilicate iron, 3-6 parts of sodium carboxymethylcellulose, 5-7 parts of activated carbon, 1-2 parts of bentonite and 2-4 parts of fly ash. The flocculant has the advantages of quick flocculation reaction, shortened production period, large flocculating body particles, easy separation and less total glycoside loss.
Description
Technical Field
The invention relates to the technical field of flocculating agents, and particularly relates to a flocculating agent for stevioside extraction.
Background
Flocculation is one of the important processes for extracting the stevia rebaudiana sugar, and can remove macromolecular impurities in the process of extracting the stevia rebaudiana sugar and improve the purity of the stevia rebaudiana sugar.
The existing flocculating agent of stevia rebaudiana sugar at home and abroad is inorganic salt, and the most common flocculating agent is FeSO4、FeCl2、Fe2(SO4)3、FeCl3、AlK(SO4)2·12H2O, etc., the inorganic salt flocculant can not completely precipitate micromolecule pectin substances in the stevia rebaudiana extract, thus affecting the purity of the stevia rebaudiana sugar and the adsorption capacity and regeneration capacity of the adsorption resin, and the flocculant is precipitated by lime water, thus increasing the load of the desalting resin and increasing the production cost. In addition, the traditional chemical impurity removal method is convenient and practical, but has the defects of slow flocculation reaction, fine flocculating constituent particles and the like, and the cycle of flocculation reaction and filter pressing clarification is longer.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the flocculating agent for extracting stevioside, which has the advantages of quick flocculation reaction, shortened production period, large flocculating body particles, easy separation and less total glycoside loss.
The invention provides a stevioside extraction flocculant which comprises the following raw materials in parts by weight: 5-9 parts of chitosan, 15-25 parts of lignin, 10-18 parts of ammonium persulfate, 20-25 parts of polyaluminum ferric sulfate, 22-24 parts of aluminum citrate, 2-7 parts of magnesium sulfate, 1-4 parts of calcium chloride, 15-25 parts of polysilicate iron, 3-6 parts of sodium carboxymethylcellulose, 5-7 parts of activated carbon, 1-2 parts of bentonite and 2-4 parts of fly ash.
Further, the chitosan is modified chitosan, and the preparation method of the modified chitosan comprises the following steps: soaking chitosan in 95% ethanol for 2-5h, transferring into a reactor, adding vanillin according to the mass ratio of vanillin to chitosan of 2-5: 1-4, stirring and refluxing in water bath with water as a solvent, adding a 10% diluted sodium hydroxide solution, filtering and cleaning, extracting with acetone, removing unreacted vanillin and other impurities, and drying to obtain vanillin modified chitosan.
Furthermore, vanillin is added according to the mass ratio of 3: 3.5 of vanillin and chitosan.
Further, the temperature of the water bath is 60-85 ℃, the reaction time in the reactor is 10-24h, and the pH value of the reaction solution is 4-6.5.
Further, the temperature of the water bath is 75 ℃, the reaction time in the reactor is 16h, and the pH of the reaction solution is 5.
Further, the preparation method of the polymeric aluminum ferric sulfate comprises the following specific steps: (1) putting 50-60g of ferrous sulfate heptahydrate into a beaker, adding distilled water and stirring to form uniform dilute pasty ferrous sulfate mixed solution; then 3-4mL of 98% concentrated H was added slowly with stirring2SO4Acidifying, and adjusting the pH of the mixed solution to 0.6-1.0; (2) adding 3.5-4.3g of sodium chlorate into the liquid prepared in the step (1) while stirring for oxidation; meanwhile, stirring at a low speed, and when uniform liquid is formed and no bubbles appear, stirring; (3) weighing aluminum sulfate according to the molar ratio of AL/Fe of 1: 11-1: 9, adding distilled water for dissolving, adding the aluminum sulfate into the ferrous sulfate mixed solution in the step (2) after dissolving, and simultaneously stirring uniformly at a low speed; (4) putting the ferrous sulfate mixed solution into a water bath kettle, and controlling the water bath temperature to be 60-80 ℃; starting the stirrer, and stirring at a low speed for 30-60 min; in the polymerization reaction process, H is added according to the proportion that the molar ratio of P/Fe is 0.1-0.33PO4As a stabilizer; (5) stirring for 20-45min, adding small amount of Na after the liquid is uniform2CO3Adjusting the alkalization degree to 0.3; (6) and after stirring is finished, taking out the product, standing for 24 hours to obtain the product, evaporating water, and drying to obtain the polymeric aluminum ferric sulfate.
Further, the raw materials comprise the following components in parts by weight: 5.2-6.3 parts of chitosan, 15.1-18.9 parts of lignin, 11-15.2 parts of ammonium persulfate, 21.3-23.2 parts of polymeric aluminum ferric sulfate, 22.4-23 parts of aluminum citrate, 3.1-5.2 parts of magnesium sulfate, 1.5-2.4 parts of calcium chloride, 16.4-19.5 parts of polysilicate iron, 3.5-4.4 parts of sodium carboxymethyl cellulose, 5.8-6.5 parts of activated carbon, 1.1-1.5 parts of bentonite and 2.3-2.9 parts of fly ash.
Further, the raw materials comprise the following components in parts by weight: 7.2-8.9 parts of chitosan, 21.2-24.7 parts of lignin, 15.3-17.5 parts of ammonium persulfate, 23.5-24.6 parts of polymeric aluminum ferric sulfate, 23.1-23.5 parts of aluminum citrate, 3.4-6 parts of magnesium sulfate, 3-3.5 parts of calcium chloride, 22-23.8 parts of polysilicate iron, 4.4-5.6 parts of sodium carboxymethyl cellulose, 6.1-6.5 parts of activated carbon, 1.3-1.85 parts of bentonite and 3-3.7 parts of fly ash.
The preparation method comprises the following steps: the composite material is prepared by uniformly mixing chitosan, lignin, ammonium persulfate, polymeric aluminum ferric sulfate, aluminum citrate, magnesium sulfate, calcium chloride, polysilicate iron, sodium carboxymethylcellulose, activated carbon, bentonite and fly ash.
The invention optimizes the components and content to obtain the flocculant which greatly improves the flocculation effect, is easy to separate and has less total glycoside loss.
The method adopts chitosan, lignin and polymeric aluminum ferric sulfate as macromolecular flocculant to quickly connect a large amount of non-glycoside organic and inorganic impurities in the stevia rebaudiana water extract to form a flocculating constituent, then the flocculating constituent is settled, aluminum citrate forms a precipitate under an alkaline condition, and the flocculating constituent is matched with activated carbon, bentonite and fly ash, so that the flocculating constituent volume is increased, the flocculating constituent settling speed can also be increased, and the activated carbon, the bentonite and the fly ash can adsorb a large amount of chlorophyll, pigment, inorganic salt and other impurities in the stevia rebaudiana water extract in the settling process, thereby playing a role in decoloring and desalting, greatly improving the efficiency of the stevioside impurity removal process and shortening the production period of the impurity removal process.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A flocculating agent for stevioside extraction comprises the following raw materials in parts by weight: 6.6 parts of chitosan, 18.5 parts of lignin, 15.8 parts of ammonium persulfate, 23 parts of polymeric aluminum ferric sulfate, 23.5 parts of aluminum citrate, 4.2 parts of magnesium sulfate, 3.3 parts of calcium chloride, 18.2 parts of polysilicate iron, 3.6 parts of sodium carboxymethylcellulose, 5.5 parts of activated carbon, 1.45 parts of bentonite and 2.8 parts of fly ash.
The preparation method of the polymeric aluminum ferric sulfate comprises the following specific steps: (1) putting 55g of ferrous sulfate heptahydrate into a beaker, adding distilled water and stirring to form uniform dilute pasty ferrous sulfate mixed solution; then 3mL of 98% concentrated H were slowly added with stirring2SO4Acidifying, and adjusting the pH of the mixed solution to 1.0; (2) adding 3.8g of sodium chlorate into the liquid prepared in the step (1) while stirring for oxidation; meanwhile, stirring at a low speed, and when uniform liquid is formed and no bubbles appear, stirring; (3) in an Al/Fe molar ratio ofWeighing aluminum sulfate, adding distilled water for dissolving, adding the aluminum sulfate into the ferrous sulfate mixed solution in the step (2) after dissolving, and simultaneously stirring uniformly at a slow speed; (4) putting the ferrous sulfate mixed solution into a water bath kettle, and controlling the water bath temperature to be 75 ℃; starting a stirrer, and stirring for 45min at a low speed; during the polymerization, H is added in a proportion of 0.2 of the molar ratio of P/Fe3PO4As a stabilizer; (5) stirring for 28min, adding small amount of Na after the liquid is uniform2CO3Adjusting the alkalization degree to 0.3; (6) after stirring, taking out the product, standing for 24 hours to obtain the product, evaporating water and drying to obtain the polymeric aluminum ferric sulfate.
Example 2
A flocculating agent for stevioside extraction comprises the following raw materials in parts by weight: 7.3 parts of chitosan, 18.4 parts of lignin, 16.6 parts of ammonium persulfate, 23.5 parts of polymeric aluminum ferric sulfate, 23 parts of aluminum citrate, 3.5 parts of magnesium sulfate, 2.6 parts of calcium chloride, 19.6 parts of polysilicate iron, 3.9 parts of sodium carboxymethylcellulose, 6.6 parts of activated carbon, 1.25 parts of bentonite and 3.4 parts of fly ash.
The chitosan is modified chitosan, and the preparation method of the modified chitosan comprises the following steps: soaking chitosan in 95% ethanol for 3h, transferring into a reactor, adding vanillin according to the mass ratio of vanillin to chitosan of 2: 3, stirring and refluxing in water bath by taking water as a solvent, adding a 10% diluted sodium hydroxide solution, filtering and cleaning, extracting with acetone, removing unreacted vanillin and other impurities, and drying to obtain vanillin modified chitosan, wherein the water bath temperature is 70 ℃, the reaction time in the reactor is 16h, and the pH of the reaction solution is 5.
The preparation method of the polymeric aluminum ferric sulfate comprises the following specific steps: (1) putting 54g of ferrous sulfate heptahydrate into a beaker, adding distilled water and stirring to form uniform dilute pasty ferrous sulfate mixed solution; then 3.6mL of 98% concentrated H was added slowly with stirring2SO4Acidifying, and adjusting the pH of the mixed solution to 0.8; (2) adding 3.8g of sodium chlorate into the liquid prepared in the step (1) while stirring for oxidation; meanwhile, stirring at a low speed, and when uniform liquid is formed and no bubbles appear, stirring; (3) weighing aluminum sulfate according to the molar ratio of AL to Fe of 1:10, addingDissolving by distilled water, adding into the ferrous sulfate mixed solution in the step (2) after dissolving, and simultaneously stirring uniformly at a slow speed; (4) putting the ferrous sulfate mixed solution into a water bath kettle, and controlling the water bath temperature to be 75 ℃; starting the stirrer, and stirring at a low speed for 40 min; during the polymerization, H is added in a proportion of 0.2 of the molar ratio of P/Fe3PO4As a stabilizer; (5) stirring for 30min, adding small amount of Na after the liquid is uniform2CO3Adjusting the alkalization degree to 0.3; (6) after stirring, taking out the product, standing for 24 hours to obtain the product, evaporating water and drying to obtain the polymeric aluminum ferric sulfate.
Example 3
A flocculating agent for stevioside extraction comprises the following raw materials in parts by weight: 6.5 parts of chitosan, 17 parts of lignin, 14.2 parts of ammonium persulfate, 23 parts of polymeric aluminum ferric sulfate, 21.3 parts of aluminum citrate, 3.6 parts of magnesium sulfate, 2.4 parts of calcium chloride, 18.1 parts of polysilicate iron, 4.3 parts of sodium carboxymethylcellulose, 6.2 parts of activated carbon, 1.44 parts of bentonite and 3.4 parts of fly ash.
The chitosan is modified chitosan, and the preparation method of the modified chitosan comprises the following steps: soaking chitosan in 95% ethanol for 4h, transferring into a reactor, adding vanillin according to the mass ratio of vanillin to chitosan of 3: 2, stirring and refluxing in water bath by using water as a solvent, adding a 10% diluted sodium hydroxide solution, filtering and cleaning, extracting with acetone, removing unreacted vanillin and other impurities, and drying to obtain vanillin modified chitosan. The temperature of the water bath is 75 ℃, the reaction time in the reactor is 16h, and the pH value of the reaction solution is 6.
The preparation method of the polymeric aluminum ferric sulfate comprises the following specific steps: (1) putting 55g of ferrous sulfate heptahydrate into a beaker, adding distilled water and stirring to form uniform dilute pasty ferrous sulfate mixed solution; then 3.2mL of 98% concentrated H was added slowly with stirring2SO4Acidifying, and adjusting the pH of the mixed solution to 0.8; (2) adding 3.8g of sodium chlorate into the liquid prepared in the step (1) while stirring for oxidation; meanwhile, stirring at a low speed, and when uniform liquid is formed and no bubbles appear, stirring; (3) weighing aluminum sulfate according to the molar ratio of AL to Fe of 1:11, adding distilled water for dissolving, and dissolvingThen adding the mixture into the ferrous sulfate mixed solution obtained in the step (2), and simultaneously stirring the mixture uniformly at a low speed; (4) putting the ferrous sulfate mixed solution into a water bath kettle, and controlling the water bath temperature to be 72 ℃; starting the stirrer, and stirring at a low speed for 40 min; during the polymerization, H was added in a proportion such that the molar ratio P/Fe was 0.253PO4As a stabilizer; (5) stirring for 40min, adding small amount of Na after the liquid is uniform2CO3Adjusting the alkalization degree to 0.3; (6) after stirring, taking out the product, standing for 24 hours to obtain the product, evaporating water and drying to obtain the polymeric aluminum ferric sulfate.
The samples 1-3 were added to stevia aqueous extract for flocculation, and polyacrylamide was used as a flocculant in the control group. Placing 200mL stevia rebaudiana water extract in a water bath at 45 deg.C, stirring at 45rpm for 15min, adding flocculant, adjusting pH to 8-9, standing for 40min, and filtering to obtain clarified stevia rebaudiana water extract. Collecting the water extractive solution and clarified water extractive solution of stevia rebaudiana Bertoni of experimental group and control group. When the content of the stevioside is measured by referring to a base capacity method in national stevioside standard GB8270-2014, the stevioside loss rate of examples 1-3 is below 3 percent, and the stevioside loss rate of a control group is 8 percent.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The stevioside extraction flocculant is characterized by comprising the following raw materials in parts by weight: 5-9 parts of chitosan, 15-25 parts of lignin, 10-18 parts of ammonium persulfate, 20-25 parts of polyaluminum ferric sulfate, 22-24 parts of aluminum citrate, 2-7 parts of magnesium sulfate, 1-4 parts of calcium chloride, 15-25 parts of polysilicate iron, 3-6 parts of sodium carboxymethylcellulose, 5-7 parts of activated carbon, 1-2 parts of bentonite and 2-4 parts of fly ash.
2. The stevioside extraction flocculant of claim 1, wherein the chitosan is modified chitosan prepared by the following steps: soaking chitosan in 95% ethanol for 2-5h, transferring into a reactor, adding vanillin according to the mass ratio of vanillin to chitosan of 2-5: 1-4, stirring and refluxing in water bath with water as a solvent, adding a 10% diluted sodium hydroxide solution, filtering and cleaning, extracting with acetone, removing unreacted vanillin and other impurities, and drying to obtain vanillin modified chitosan.
3. The stevioside extraction flocculant of claim 2, wherein vanillin is added in a mass ratio of vanillin to chitosan of 3: 3.5.
4. The flocculant for stevioside extraction according to claim 2 or 3, wherein the water bath temperature is 60 to 85 ℃, the reaction time in the reactor is 10 to 24 hours, and the pH of the reaction solution is 4 to 6.5.
5. The flocculant for stevioside extraction according to one of claims 1 to 3, wherein the polymeric aluminum ferric sulfate is prepared by the following specific steps: (1) putting 50-60g of ferrous sulfate heptahydrate into a beaker, adding distilled water and stirring to form uniform dilute pasty ferrous sulfate mixed solution; then 3-4mL of 98% concentrated H was added slowly with stirring2SO4Acidifying, and adjusting the pH of the mixed solution to 0.6-1.0; (2) adding 3.5-4.3g of sodium chlorate into the liquid prepared in the step (1) while stirring for oxidation; meanwhile, stirring at a low speed, and when uniform liquid is formed and no bubbles appear, stirring; (3) weighing aluminum sulfate according to the molar ratio of AL/Fe of 1: 11-1: 9, adding distilled water for dissolving, adding the aluminum sulfate into the ferrous sulfate mixed solution in the step (2) after dissolving, and simultaneously stirring uniformly at a low speed; (4) putting the ferrous sulfate mixed solution into a water bath kettle, and controlling the water bath temperature to be 60-80 ℃; starting the stirrer, and stirring at a low speed for 30-60 min; in the polymerization reaction process, H is added according to the proportion that the molar ratio of P/Fe is 0.1-0.33PO4As a stabilizer; (5) stirring for 20-45min, adding small amount of Na after the liquid is uniform2CO3Adjusting the alkalization degree to 0.3; (6) and after stirring is finished, taking out the product, standing for 24 hours to obtain the product, evaporating water, and drying to obtain the polymeric aluminum ferric sulfate.
6. The stevioside extraction flocculant of claim 4, wherein the water bath temperature is 75 ℃, the reaction time in the reactor is 16h, and the pH of the reaction solution is 5.
7. The stevioside extraction flocculant of claims 1-6, which comprises the following raw materials in parts by weight: 5.2-6.3 parts of chitosan, 15.1-18.9 parts of lignin, 11-15.2 parts of ammonium persulfate, 21.3-23.2 parts of polymeric aluminum ferric sulfate, 22.4-23 parts of aluminum citrate, 3.1-5.2 parts of magnesium sulfate, 1.5-2.4 parts of calcium chloride, 16.4-19.5 parts of polysilicate iron, 3.5-4.4 parts of sodium carboxymethyl cellulose, 5.8-6.5 parts of activated carbon, 1.1-1.5 parts of bentonite and 2.3-2.9 parts of fly ash.
8. The stevioside extraction flocculant of claims 1-6, which comprises the following raw materials in parts by weight: 7.2-8.9 parts of chitosan, 21.2-24.7 parts of lignin, 15.3-17.5 parts of ammonium persulfate, 23.5-24.6 parts of polymeric aluminum ferric sulfate, 23.1-23.5 parts of aluminum citrate, 3.4-6 parts of magnesium sulfate, 3-3.5 parts of calcium chloride, 22-23.8 parts of polysilicate iron, 4.4-5.6 parts of sodium carboxymethyl cellulose, 6.1-6.5 parts of activated carbon, 1.3-1.85 parts of bentonite and 3-3.7 parts of fly ash.
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