CN1861638A - Process for preparing pectin and heavy metallic ion adsorber by soybean peel combined production - Google Patents
Process for preparing pectin and heavy metallic ion adsorber by soybean peel combined production Download PDFInfo
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Abstract
A process for preparing pectin and heavy metal ion adsorbent from the peel of soybean seed includes such steps as cleaning said peels, extracting by complexing agent, decoloring by activated carbon or cold alkali, depositing in acidic solution, solid-liquid separation for removing acidic water, depositing pectin in organic solvent, filtering, leaching by solvent, removing solvent, drying, pulverizing to obtain pectin, pretreating the used peels or raw peels by metal chelating agen and diluted alkali solution, treating by acid and surfactant, immersing in water, drying and pulverizing to obtain the heavy metal ion adsorbent.
Description
One, technical field: the present invention relates to a kind of method for preparing pectin and adsorbent for heavy metal, especially is main raw material with the soybean peel, extracts the method for pectin and adsorbent for heavy metal by deep processing.
Two, background technology: the main products of soyabean processing industry is soya-bean oil and various soybean protein both at home and abroad at present.In the soyabean processing process, at first to peel, take off selected and sorting preprocessings such as plumule, with quality and the yield of guaranteeing soya-bean oil and various soybean proteins.Soybean peel is the by product of the amount maximum that produces in the soybean deep-processing process, accounts for 8～10% of soybean weight.Soybean peel nutritive value lower (crude protein content 11%, crude fiber content 36%, crude fat content 1%), be difficult for absorbing for animal digestion, add and contain a large amount of antinutritional factor---phytic acid, even reluctantly as the feed of ruminating animals such as ox, sheep, utility value is not high yet.Pectin has good pectisation, emulsifying effect, adsorption, is widely used in fields such as the production of food, medicine, makeup and water conditioning.
At present, the starting material that extract pectin both at home and abroad mainly are materials such as peel of Citrus reticulata Blanco, apple residue, beet pulp, the extraction process of pectin mainly is to utilize dilute acid soln that protopectin is hydrolyzed to water soluble pectin matter and transfers to aqueous phase, utilizes pectin to be insoluble to ethanol, acetone etc. and water miscible organic solvent again or produces the flocculation precipitating and extract when some ionizable metal salts exist.Its technical process is: raw materials pretreatment → acid solution hydrolysis → filtration → decolouring → de-ash → concentrate → precipitating → drying → pulverizing → standardization → finished product.Key in the process for producing pectin is extraction and separates two steps.
In recent years, abroad begin with the soybean peel is the research and development that raw material begins to extract pectin, the method of representative preparing pectin by soybean seed coat is: (1) raw materials pretreatment: soybean peel (through sieving and selection by winnowing) is a raw material, stirred 1 hour with 12 times of water of skin of beancurd weight, through flotation and washing, inclining showy part, uses after drip washing drains, and mixes to remove impurity such as silt.(2) soybean peel hydrolysis: take the acid heat hydrolysis, once extract the extracted twice method of putting forward with slag.Inorganic acid concentration represents that with mole with the solution dilution of 6 mol concentration, under the acidometer monitoring, fine adjustment stirs hydrolysis and lixiviate certain hour to nominal pH value under certain bath raio again; And the variation of monitoring pH value in insulation reaction is extracted.(3) neutralization: the NaOH solution with 4 mol is adjusted the pH value, reduces acidity, in order to avoid remain in strong acidic environment for a long time, causes excessive hydrolysis, influences pectin yield and quality product.(4) solid-liquid separation: adopt suction method, carry out in B, vacuum pump provides negative pressure.(5) decolouring: activated carbon adsorption decolouring.Solution is preheating to 82 ℃, and pH is transferred to 2.5, and 2～5% (weight/volume) of pressing solution add activated carbon, stirs insulation down and handles suction filtration deactivation carbon in the B 30 fens.(6) concentrate: carried out normal pressure, decompression (65 ℃) and ultrafiltration and concentration respectively.(7) solvent deposition: solvent deposition is one of method of effectively isolating pectin substance, and with methyl alcohol, ethanol and acetone, flocculation and effect of settling are similar.(8) recycling precipitate: adopt suction method, again through aqueous ethanol drip washing, dense ethanol dehydration impurity elimination.(9) product obtains: precipitation, crushed after being dried, cross 100 mesh standard sieves.It is the technical feasibility that raw material extracts pectin that this method has solved soybean peel from theory, but exists output efficiency low in the actual application, the problem that technique controlling difficulty is high.
Three, summary of the invention: purpose of the present invention is exactly the defective that exists at prior art, provides a kind of soybean peel coproduction to prepare the method for pectin and adsorbent for heavy metal.This method is extracted pectin according to being to contain in the soybean peel with calcium ions and magnesium ions etc. to be the pectin substance of bonding state, thereby can not be water-soluble.Utilize complexing agent to compete and combine, make with the pectin of calcium ions and magnesium ions bonding state freely, become water-soluble state, thereby make pectin enter extracting solution to reach the purpose of extracting pectin with calcium ions and magnesium ions.Utilize the isolating skin of beancurd slag in extraction back directly to prepare adsorbent for heavy metal simultaneously.
Its technical scheme comprises:
(1) prepare the method for pectin:
(1) preparation of raw material and pre-treatment: soybean peel need add 10-20 times of normal-temperature water through after selected, the impurity elimination, adjusts pH value to 11, stirs 20-40 minute water washing cleaning;
(2) soy pectin extracts: take network and agent once to extract method with extracted twice; The complexing agent consumption is 0.5%-2.0% by the concentration that is made into certain solution, and pH value 7.5-11.0 stirred 50-70 minute, and monitors the variation of pH value under 65 ℃～95 ℃ conditions of temperature;
(3) extracting liquid decoloration: activated carbon adsorption decolouring and two kinds of methods of cold alkali aggregate expansion;
(4) pectin precipitation: adjust pH 1.5～4.5, heavy 15-25 minute of acid;
(5) solid-liquid separation: adopt filter press technique deacidification water;
(6) pickling after the press filtration: under pH value 1.5～4.5 conditions, pickling 10-25 minute;
(7) alcohol/ammonia solution washing: adopt concentration 40-60% organic alcohol solvent with the pectin post precipitation, with ammoniacal liquor adjust pH 8.0-9.0,30 minutes time;
(8) sediment separate out reclaims: the pectin of solvent deposition gained is used 60%, 70% and 95～98% water-containing solvent drip washing successively;
(9) product obtains: precipitation, crushed after being dried.
Extract the used complexing agent of soy pectin and comprise Sodium hexametaphosphate 99, EDTA; The selection of organic alcohol solvent comprises several solvents such as methyl alcohol, ethanol, propyl alcohol, Virahol, acetone, is advisable with food grade ethanol.
(2) prepare the method for adsorbent for heavy metal:
With soybean peel or the dried skin of beancurd of drying after extracting pectin as raw material, through metal chelator, diluted alkaline pre-treatment, after organic acid and inorganic weak acid and tensio-active agent processing, water embathes removes residual acid again, drying, pulverizing obtain pulverous adsorbent for heavy metal.
The organic acid of preparation adsorbent for heavy metal is a citric acid, and inorganic weak acid is a phosphoric acid, and drying temperature is between 70-95 ℃.(whether please check this part correct)
On the basis of such scheme, compare Journal of Sex Research and experiment with regard to the relevant technologies parameter, the following raising and the recovery rate and the quality product concrete measure that improve product proposed.
1, cleaning is to the influence of pectin quality.Cleaning helps improving the quality of products, and can effectively improve product color, reduce ash.
2, the skin of beancurd granularity is to the influence of pectin yield.Taking all factors into consideration the each side factor adopts the soybean peel raw material of not pulverizing directly to use.
3. extract of the influence of the used complexing agent kind of soy pectin: adopt multiple complexing agents such as Sodium hexametaphosphate 99, EDTA to combine respectively with calcium, magnesium ion in the soybean peel to yield and quality product.Take all factors into consideration factor EDTA such as environmental protection, price, source, effect and certain advantage is arranged as complexing agent.Find also in the experiment that the pH value of suitably regulating extracting solution can make the extraction yield increase.
In the extracting solution complexing agent concentration to the influence of yield: network and agent solution with different concns extract soy pectin, found that complexing agent concentration is lower than 0.2, DeGrain, yield is on the low side, the complexing agent concentration height, yield is steady, but that concentration is higher than is 0.8 no longer in rising trend.
5. extract the influence of temperature: carried out 15 ℃ of room temperatures, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 95 ℃, 100 ℃ extraction pectin experiments down respectively to pectin yield, found that: temperature is low, yield is low, but be not the temperature height, yield is just corresponding high, 80 ℃～90 ℃ are extracted down, recovery rate is similar, and the yield of extracting under the condition more than 95 ℃ descends again on the contrary to some extent, and the pectin viscosity in aqueous solution of allotting also decreases.May be that the pectin that causes lixiviate to go out under stronger heat condition is further degraded, molecule diminishes, and is difficult to sedimentation.During with extract with EDTA pectin, temperature to the influence degree of yield and rule and with acid system extract similar.
6. bath raio is to the influence of pectin yield and quality product: other condition is fixed, extract experiment by 5: 1,10: 1,15: 1,20: 1,25: 1 condition of bath raio, found that: bath raio is 5: 1 o'clock, can not soak soybean peel fully, bath raio is 10: 1 above could immersions fully; It is low that bath raio is crossed low yield, the solvent deposition thing be cotton-shaped and thread, the too high yield of bath raio is also lower, and the viscosity of gained pectin solution is poor slightly.8: 1,15: 1 of more suitable bath raioes further relatively, the result with 10: 1～12: 1 for the suitableeest.
7. extraction time is to the influence of pectin yield: other condition is fixed, and extraction time is a variable, does series of experiments.The result is: the time is too short, and hydrolyzed pectin and lixiviate in the soybean peel are incomplete, and yield is obviously on the low side.Overlong time, the pectin in the skin of beancurd excessively is hydrolyzed into small molecules, add solvent after, be difficult to precipitation, yield also decreases, and the water-soluble viscosity of gained pectin is relatively poor.Extraction time conforms to trend with the result who extracts test with acid system with the relation of pectin yield.In 60 minutes, along with the increase of time, yield rises, and is advisable time expand (90 minutes) yield slightly decline on the contrary again with 60 minutes.
8. the relation of sour heavy pH value and pectin yield: other condition is fixed, and the heavy pH value of acid is a variable, does series of experiments.The result is: the heavy pH value of acid is low excessively, and the pectin precipitation in the soybean peel extracting solution is incomplete, and pectin substance is all with fluid loss, and yield is obviously on the low side.With pH value 1.5～4.5 is good.
9. the relation of pickling pH value and pectin yield: get the acid of the isodose pectin after heavy, clean with the sour water of different pH values, relatively cleaning performance discovery pH hangs down excessively that to have part pectin water-soluble, causes yield on the low side; PH is too high, and is unfavorable to equipment and technology.To clean better with the similar acidified water of the heavy pH value of acid.
10. with the selection of the mixable organic solvent of water: pectin is insoluble to ethanol etc. and the mixable organic solvent of water, therefore it can be precipitated out in concentrated solution with this class organic solvent.Relatively cross several solvents such as methyl alcohol, ethanol (dehydrated alcohol and industrial alcohol), propyl alcohol, Virahol, acetone in the test, find that the sedimentation effect difference is little.Consider source, price, the difficulty or ease of recovery and the composite factors such as specification requirement that are used for the additive of food of toxicity, propyl alcohol and the Virahol of methyl alcohol, still select for use the food grade ethanol of fermentative Production to be advisable.
According to the new extraction conditions that the laboratory is optimized, adopt the new technology route after improving to carry out amplification and revision test, continuous 7 batches of extract with EDTA pectin method setting-out test-results are as shown in the table:
Annotate: all batches test is only through once extracting, if can reach 14～15% through pectin yield after the second extraction
| Batch | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Sample heavy (gram) | 200 | 200 | 400 | 400 | 400 | 400 | 400 |
| Pectin heavy (gram) | 22.375 | 23.087 | 47.048 | 44.091 | 46.016 | 44.16 | 47.03 |
| Yield (%) | 11.19 | 11.54 | 11.76 | 11.02 | 11.50 | 11.04 | 11.76 |
The present invention extracts pectin and compares with the traditional method of extracting pectin from materials such as peel of Citrus reticulata Blanco, apple residue, beet pulp from soybean peel, have following advantage at least: (1), soybean peel are as the byproduct of soyabean processing enterprise, and low price is collected easily; (2), soybean peel does not need further to process just can to store and transport; (3), the development trend of prediction low sugar, heath food low in calories and functional food and the increase of the market requirement, the natural low-ester pectin that obtains in the soybean peel (calcium gelation) will become traditional pectin (high ester pectins such as citrus pectin, apple pectin, high sugared gelation) pectin new variety in addition.In addition, can also utilize the isolated skin of beancurd slag of extraction pectin directly to prepare adsorbent for heavy metal in the solution of the present invention.Prove through laboratory and pilot experiment that from technical scheme of the present invention extraction and separating technology are rationally ripe more, have good application prospects.
Four, description of drawings: accompanying drawing is a process flow sheet of the present invention.
Five, specific embodiment:
With reference to accompanying drawing, specific embodiments of the present invention comprises:
(1) scheme of preparation pectin is:
(1) preparation of raw material and pre-treatment: soybean peel need add 15 times of normal-temperature water through after selected, the impurity elimination, adjusts pH value to 11, stirs 30 minutes water washing cleanings.
(2) soy pectin extracts: take network and agent once to extract method with extracted twice.Complexing agent is 1.0% with Sodium hexametaphosphate 99 or EDTA by the concentration that is made into certain solution, and pH value 9.5 stirred 60 minutes, and monitors the variation of pH value under 85 ℃ of conditions of temperature.
(3) extracting liquid decoloration: activated carbon adsorption decolouring and two kinds of methods of cold alkali aggregate expansion.
(4) pectin precipitation: adjust pH 2.5, heavy 20 minutes of acid.
(5) solid-liquid separation: adopt suction method deacidification water.
(6) pickling after the press filtration: under pH value 2.5 conditions, pickling 15 minutes.
(7) carry out alcohol/ammonia solution washing after the press filtration once more: adopt concentration 50% alcohol solvent with the pectin post precipitation, with ammoniacal liquor adjust pH 8.5,30 minutes time;
(8) sediment separate out reclaims: the pectin of solvent deposition gained is used 60%, 70% and 95% water-containing solvent drip washing successively;
(9) isolating product obtains finished product after screw extrusion, drying, pulverizing, packing.
(2) scheme of preparation adsorbent for heavy metal is:
With soybean peel or the dried skin of beancurd of drying after extracting pectin as raw material, through metal chelator, diluted alkaline pre-treatment, after organic acid and inorganic weak acid and tensio-active agent processing, water embathes removes residual acid again, drying, pulverizing obtain pulverous adsorbent for heavy metal.The organic acid of preparation adsorbent for heavy metal is a citric acid, and inorganic weak acid is a phosphoric acid, and drying temperature is at 90 ℃.
Claims (4)
1, a kind of soybean peel coproduction prepares the method for pectin and adsorbent for heavy metal, it is characterized in that comprising:
(1) prepare the method for pectin:
(1) preparation of raw material and pre-treatment: soybean peel need add 10-20 normal-temperature water doubly through selected after the impurity elimination, adjust pH value to 11, stirs 20-40 minute water washing cleaning;
(2) soy pectin extracts: take network and agent once to extract method with extracted twice, network and agent consumption are 0.5%-2.0% by the concentration that is made into certain solution, pH value 7.5-11.0 stirred 50-70 minute, and monitored the variation of pH value under 65 ℃ of-95 ℃ of conditions of temperature;
(3) extracting liquid decoloration: activated carbon adsorption decolouring and cold alkali aggregate expansion method:
(4) pectin precipitation: transfer pH value 1.5-4.5, heavy 15-25 minute of acid;
(5) solid-liquid separation: adopt filter press technique deacidification water;
(6) pickling after the press filtration: under pH value 1.5-4.5 condition, pickling 10-25 minute;
(7) alcohol/ammonia solution washing: adopt concentration 40-60% organic alcohol solvent with the pectin post precipitation, transfer pH value 8.0-9.0,30 minutes time with ammoniacal liquor;
(8) sediment separate out reclaims: the pectin of solvent deposition gained is used 60%, 70% and 95～98% water-containing solvent drip washing successively;
(9) product obtains: precipitation, crushed after being dried;
(2) prepare the method for adsorbent for heavy metal:
With soybean peel or the dried skin of beancurd of drying after extracting pectin as raw material, through metal chelator, diluted alkaline pre-treatment, join or after inorganic weak acid and tensio-active agent handled, water embathes removed residual acid through organic again, drying, pulverizing obtain pulverous adsorbent for heavy metal.
2, soybean peel coproduction according to claim 1 prepares the method for pectin and adsorbent for heavy metal, it is characterized in that: extract the used complexing agent of soy pectin and comprise Sodium hexametaphosphate 99, EDTA; The selection of organic alcohol solvent comprises several solns such as methyl alcohol, ethanol, propyl alcohol, Virahol, acetone.
3, soybean peel coproduction according to claim 1 prepares the method for pectin and adsorbent for heavy metal, it is characterized in that: the organic acid of preparation adsorbent for heavy metal is a citric acid, and inorganic weak acid is a phosphoric acid, and drying temperature is between 70-95 ℃.
4, the method for preparing pectin by soybean seed coat according to claim 2 is characterized in that: the selection of organic alcohol solvent is advisable with food grade ethanol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2011137585A1 (en) * | 2010-05-05 | 2011-11-10 | Empire Technology Development Llc | Method for removing metals from a metal-containing solution by using legume plants |
| CN102492054A (en) * | 2011-12-06 | 2012-06-13 | 渤海大学 | Preparation method of soybean episperm pectin gel polysaccharide |
| CN105441081A (en) * | 2015-12-14 | 2016-03-30 | 缪琼华 | Eluting solution capable of restoring heavy metal-contaminated soil |
| CN105542779A (en) * | 2015-12-14 | 2016-05-04 | 缪琼华 | Preparation method of leaching liquid for repairing heavy metal polluted soil |
| CN107321334A (en) * | 2017-08-30 | 2017-11-07 | 齐鲁工业大学 | A kind of preparation method of modified gingko episperm alginate microsphere adsorbent |
| CN107335409A (en) * | 2017-08-29 | 2017-11-10 | 齐鲁工业大学 | A kind of method that gingko episperm prepares sorbing material |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001038400A2 (en) * | 1999-11-22 | 2001-05-31 | Crandall Philip G | Isolation of pectin from soybeans |
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2005
- 2005-10-25 CN CNB2005101044582A patent/CN100422217C/en active Active
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011137585A1 (en) * | 2010-05-05 | 2011-11-10 | Empire Technology Development Llc | Method for removing metals from a metal-containing solution by using legume plants |
| CN102869614A (en) * | 2010-05-05 | 2013-01-09 | 英派尔科技开发有限公司 | Method for removing metals from a metal-containing solution by using legume plants |
| CN102869614B (en) * | 2010-05-05 | 2015-04-22 | 英派尔科技开发有限公司 | Method for removing metals from a metal-containing solution by using legume plants |
| CN102492054A (en) * | 2011-12-06 | 2012-06-13 | 渤海大学 | Preparation method of soybean episperm pectin gel polysaccharide |
| CN102492054B (en) * | 2011-12-06 | 2013-08-21 | 渤海大学 | Preparation method of soybean episperm pectin gel polysaccharide |
| CN105441081A (en) * | 2015-12-14 | 2016-03-30 | 缪琼华 | Eluting solution capable of restoring heavy metal-contaminated soil |
| CN105542779A (en) * | 2015-12-14 | 2016-05-04 | 缪琼华 | Preparation method of leaching liquid for repairing heavy metal polluted soil |
| CN107335409A (en) * | 2017-08-29 | 2017-11-10 | 齐鲁工业大学 | A kind of method that gingko episperm prepares sorbing material |
| CN107321334A (en) * | 2017-08-30 | 2017-11-07 | 齐鲁工业大学 | A kind of preparation method of modified gingko episperm alginate microsphere adsorbent |
| CN107362783A (en) * | 2017-08-30 | 2017-11-21 | 齐鲁工业大学 | A kind of method that gingko episperm sorbing material is prepared using ball milling means |
| CN107321334B (en) * | 2017-08-30 | 2019-12-31 | 齐鲁工业大学 | Preparation method of modified ginkgo biloba exocarp-alginate microsphere adsorbent |
| CN107362783B (en) * | 2017-08-30 | 2020-07-31 | 齐鲁工业大学 | Method for preparing ginkgo biloba exocarp adsorbing material by adopting ball milling means |
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Effective date of registration: 20200224 Address after: 315000 No.12 Xingye Avenue, Ningbo Free Trade Zone, Ningbo City, Zhejiang Province Co-patentee after: Shandong Wan De Fu Biotechnology Co., Ltd. Patentee after: Ningbo sobao protein Technology Co., Ltd Address before: 257500, No. 187 Li River Road, Kenli County, Shandong, Dongying Patentee before: Shandong Wonderful Industrial Group Co., Ltd. |