CN1594368A - Method for producing high pure chitosan with low consumption and high yield - Google Patents
Method for producing high pure chitosan with low consumption and high yield Download PDFInfo
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- CN1594368A CN1594368A CN 200410040121 CN200410040121A CN1594368A CN 1594368 A CN1594368 A CN 1594368A CN 200410040121 CN200410040121 CN 200410040121 CN 200410040121 A CN200410040121 A CN 200410040121A CN 1594368 A CN1594368 A CN 1594368A
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Abstract
The invention discloses a method for producing high pure chitosan with low consumption and high yield, which consists of washing, filtering, squashing, water scrubbing the maggot skin, charging alkali liquor sectionwise, removing proteins twice, decolorizing, charging oxalic acid sectionwise, demanganization twice, purifying and drying.
Description
Technical field
The present invention relates to a kind of production method of chitin, relate in particular to the production method of the high yield high-purity chitin of a kind of low consumption.
Background technology
Existing from fly maggot in the method for chitin extraction, Chinese patent notification number CN1112369C discloses a kind of " method of high-purity chitin extracting from housefly maggot ", though this method relates to effective removal fly maggot mouthpart and internal organ, but the consumption of pharmaceutical chemicals consumption and energy is bigger in the production process, thereby its cost is higher, and the purity of product and yield are all not high.
Summary of the invention
The object of the present invention is to provide a kind of chitin purity>99%, maggot mouthpart and organic pigment clearance>95%, the production method of the high yield high-purity chitin that yield height and pharmaceutical chemicals consumption are few.
The contriver finds method of the present invention through test for many years: add the moisture that accounts for bright maggot weight 1/5, rotating speed is that 10000r/min can make maggot skin and internal organ and proteinic separating effect reach best.Washing maggot skin can be removed most of protein, to reduce the used amount of sodium hydroxide of deproteinization; Determine the optimum value of alkali charge, temperature, concentration of lye with orthogonal experiment, the gradation of alkaline solution adds can comparatively fully remove protein residual on the maggot skin and fat, and the alkali lye first time that can be used as the deproteinization stage after for the second time used alkali lye reclaims is reused; Potassium permanganate reacts under the alkaline environment of PH13~14, has both guaranteed to take off mouthpart and take off effectively carrying out of organic pigment, has guaranteed that again the oxalic acid reduction removes inorganic pigment; Soak the back yellow substance at oxalic acid and can separate preferably with chitin with internal organ, make product colour whiter, purity is higher; The oxalic acid first time that can be used as the demanganization stage after for the second time used oxalic acid reclaims is reused; Hydrochloric acid is also once reusable.By the repeated use of acid-base solution in this method, can reduce the usage quantity of the pharmaceutical chemicals in the inventive method to greatest extent.
The production method of a kind of high yield high-purity chitin of the present invention comprises the steps:
(1) pre-treatment: get bright maggot and clean, filter is done, and adds the tap water that accounts for bright maggot weight 1/5, places crusher jointly, with the broken 2min of 10000r/min, and washing maggot skin;
(2) deproteinization: get clean maggot skin and put into reactor, the weight concentration that the bright maggot adding of 1kg 1L reclaims is 4% NaOH solution, is incubated 2 hours down at 90 ℃~100 ℃, uninterrupted slow the stirring, filter, and then with weight concentration be 4% NaOH solution repetition aforementioned operation once;
(3) fade: the bright maggot of 1kg is 1% KMnO4 solution with 11 weight concentrations, and at room temperature soaked 3~12 hours adjusting PH13~14, washes 4-5 time;
(4) weight concentration that the bright maggot of demanganization: 1kg is reclaimed with 1L is that 1% oxalic acid soaked 3 hours, filters, and be 1% oxalic acid immersion more than 3 hours with weight concentration once more, leach oxalic acid;
(5) the bright maggot of purifying: 1kg removes by filter HCL with soaking 3 hours among the 0.4-0.6L 1mol/l HCL, is washed to neutrality;
(6) drying: centrifuge dehydration, 60 ℃ of dryings.Obtain purity>99%, ignition residue<0.5%, heavy metal (in lead)<2ppm, outward appearance is pure white, the chitin of maggot mouthpart and organic pigment clearance>95%.
Method of the present invention, the 4%NaOH solution that reclaims in (2) step is the 4%NaOH solution after using for the second time in this step.
Method of the present invention, the oxalic acid of 1% recovery in (4) step is 1% oxalic acid solution after using for the second time in this step.
Method of the present invention, the HCL in (5) step, once reusable.
As can be known from the above technical solutions, method of the present invention compared with prior art, the segmentation of soda acid adds and reuses and both guaranteed protein and fat and calcareous effectively removing, and has reduced production cost again; Potassium permanganate reacts under the alkaline environment of PH13~14, both guaranteed to take off mouthpart and take off effectively carrying out of organic pigment, guaranteed again that the oxalic acid reduction removed inorganic pigment, and soaked the back yellow substance at oxalic acid and can separate preferably with chitin with internal organ, make product colour whiter, purity is higher.Recyclable utilization behind the acid-base neutralisation of processing chitin, potassium permanganate after the processing and oxalic acid neutralization, filtration prevent soda acid discharging and heavy metal contamination.Because used chemical agent concentration and amount, reaction conditions were through the select optimum value of orthogonal experiment during method of the present invention respectively went on foot, and had both effectively reduced reagent dosage and energy consumption, had guaranteed high quality, can obtain higher yield again.
Embodiment
Below the specific embodiment of the production method by a kind of high yield high-purity chitin of the present invention is further set forth effect of the present invention.
(1) pre-treatment: get the bright maggot of 50kg and clean, filter is done, and adds the 10kg tap water, place jointly in crusher,, separate maggot skin and albumen chylema with the broken 2min of 10000r/min, washing maggot skin is removed most of protein, can reduce the used amount of sodium hydroxide of deproteinization.
(2) deproteinization: get and clean the maggot skin and put into reactor, add the 50L weight concentration and be 4% NaOH solution be incubated in 90 ℃~100 ℃ 2 hours, uninterruptedly slowly stir, filter; For the second time with new weight concentration be 4% NaOH solution repetition aforementioned operation once, can remove protein residual on the maggot skin and fat fully.The gradation of alkaline solution adds can effectively remove residual protein and fat.For the second time used alkali lye is also once reusable, and the repeated use of NaOH has reduced reagent consumption.
(3) fade: with the weight concentration of 50L is 1% KMnO4 solution (transferring pH13~14) soaking at room temperature 3~12 hours, can effectively remove insoluble impuritiess such as mouthpart, organic pigment, wash 4-5 time, and the residual KMnO4 of flush away that tries one's best is advisable.Weight concentration is that 1% KMnO4 solution can well be removed mouthpart and organic pigment under the condition of pH13~14.
(4) demanganization: with the 50L weight concentration is that 1% oxalic acid soaked 3 hours, filters; Be that 1% oxalic acid soaked more than 3 hours with new weight concentration again, leach oxalic acid.Used oxalic acid is once reusable for the second time.Oxalic acid after the use can neutralize to avoid contaminate environment with potassium permanganate.
(5) purifying: with soaking 3 hours among the 30L 1mol/lHCL, remove by filter HCL, be washed to neutrality.Hydrochloric acid is also once reusable.
(6) drying: centrifuge dehydration, 60 ℃ of dryings.Obtain purity>99%, ignition residue<0.5%, heavy metal (in lead)<2ppm, outward appearance is pure white, the chitin 0.5kg of maggot mouthpart and organic pigment clearance>95%.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (4)
1, the production method of the high yield high-purity chitin of a kind of low consumption comprises the steps:
(1) pre-treatment: get bright maggot and clean, filter is done, and adds the tap water that accounts for bright maggot weight 1/5, places crusher jointly, with the broken 2min of 10000r/min, and washing maggot skin;
(2) deproteinization: get clean maggot skin and put into reactor, the weight concentration that the bright maggot adding of 1kg 1L reclaims is 4% NaOH solution, is incubated 2 hours down at 90 ℃~100 ℃, uninterrupted slow the stirring, filter, and then with weight concentration be 4% NaOH solution repetition aforementioned operation once;
(3) fade: the bright maggot of 1kg is 1% KMnO4 solution with the 1L weight concentration, and at room temperature soaked 3~12 hours adjusting PH13~14, washes 4-5 time;
(4) weight concentration that the bright maggot of demanganization: 1kg is reclaimed with 1L is that 1% oxalic acid soaked 3 hours, filters, and be 1% oxalic acid immersion more than 3 hours with weight concentration once more, leach oxalic acid;
(5) the bright maggot of purifying: 1kg removes by filter HCL with soaking 3 hours among the 0.4-0.6L 1mol/1HCL, is washed to neutrality;
(6) drying: centrifuge dehydration, 60 ℃ of dryings.Obtain purity>99%, ignition residue<0.5%, heavy metal (in lead)<2ppm, outward appearance is pure white, the chitin of maggot mouthpart and organic pigment clearance>95%.
2, the method for claim 1, the 4%NaOH solution that reclaims in (2) step is the 4%NaOH solution after using for the second time in this step.
3, the method for claim 1, the oxalic acid of 1% recovery in (4) step is 1% oxalic acid solution after using for the second time in this step.
4, the method for claim 1, the HCL in (5) step, once reusable.
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CN 200410040121 CN1594368A (en) | 2004-06-30 | 2004-06-30 | Method for producing high pure chitosan with low consumption and high yield |
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CN 200410040121 CN1594368A (en) | 2004-06-30 | 2004-06-30 | Method for producing high pure chitosan with low consumption and high yield |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102199228A (en) * | 2010-03-30 | 2011-09-28 | 甘肃农业大学 | Preparation processes of flyblow chitin and chitosan and application of flyblow chitin in inducing trichoderma aureoviride T2 strains to produce chitinases |
WO2019115970A1 (en) * | 2017-12-15 | 2019-06-20 | Ynsect | Chitin and process for producing chitin and/or chitosan by the enzymatic and chemical pathway |
-
2004
- 2004-06-30 CN CN 200410040121 patent/CN1594368A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102199228A (en) * | 2010-03-30 | 2011-09-28 | 甘肃农业大学 | Preparation processes of flyblow chitin and chitosan and application of flyblow chitin in inducing trichoderma aureoviride T2 strains to produce chitinases |
CN102199228B (en) * | 2010-03-30 | 2013-04-17 | 甘肃农业大学 | Preparation processes of flyblow chitin and chitosan and application of flyblow chitin in inducing trichoderma aureoviride T2 strains to produce chitinases |
WO2019115970A1 (en) * | 2017-12-15 | 2019-06-20 | Ynsect | Chitin and process for producing chitin and/or chitosan by the enzymatic and chemical pathway |
FR3075205A1 (en) * | 2017-12-15 | 2019-06-21 | Ynsect | CHITINE AND PROCESS FOR OBTAINING CHITIN AND / OR CHITOSAN BY ENZYMO CHEMICAL |
US11958918B2 (en) | 2017-12-15 | 2024-04-16 | Ynsect | Chitin and process for producing chitin and/or chitosan by the enzymatic and chemical pathway |
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