CN105524189A - Method for preparing oligochitosan through self-resonating cavitation - Google Patents
Method for preparing oligochitosan through self-resonating cavitation Download PDFInfo
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
The invention relates to a method for preparing oligochitosan through self-resonating cavitation. The method is characterized in that self-resonating cavitation degradation is adopted, that is, a chitosan solution is subjected to self-resonating cavitation degradation treatment in a self-resonating cavitation device; the self-resonating cavitation device comprises a thermostatic water-bath circulation water tank, a storage tank, a pump, a self-resonating cavitation device, a pipeline for conveying the chitosan solution, a pressure gauge and a valve; the technological process of self-resonating cavitation degradation is as follows: the chitosan solution is stored in the storage tank, subjected to thermostatic treatment by the circulation water tank and conveyed by the pump to the self-resonating cavitation device for cavitation degradation, the pressure of an inlet is adjusted by the valve, the pressure is monitored by the pressure gauge, and the chitosan solution subjected to cavitation degradation flows back to the storage tank. The degradation rate by using the method is at least 40% higher than that by using a hydrodynamic cavitation device (venturi tube) to prepare oligochitosan at present, and the method has the characteristics of simplicity, easiness, low energy consumption, high efficiency and the like and has the advantage of mass industrial application.
Description
Technical field
The present invention relates to a kind of preparation method of chitosan oligomer method, particularly one utilizes self-vibration cavitation to prepare chitosan oligomer method.
Background technology
The general chitosan molecule amount obtained by de-acetyl chitin is very large, and has crystalline structure closely, and be insoluble to usual vehicle, can only be dissolved in some acidic medium, this makes the application of chitosan be subject to great restriction.In addition, research shows: the chitosan nature difference of different relative molecular mass is very large, and sometimes even can show diametrically opposite characteristic, many specific function of chitosan are only reduced at relative molecular mass and to a certain degree just show.Chitosan, through the low-molecular water-soluble chitosan that obtains of degrading, has unique, superior physiologically active and physico-chemical property, has a wide range of applications field and Development volue, thus receive much attention.
At present, degradation of chitosan method mainly contains chemical method, enzyme process and Physical.
(1) chemical method is degraded to chitosan by the method for chemistry, mainly contains: acid degradation method, NaNO
2edman degradation Edman, oxidation degradation method etc.Chemical degradative processes reacts bad control, and relative molecular mass distribution is wide, and easily to environment, product colour is darker.
(2) enzymic degradation is the method utilizing specificity or non-specific enzyme to degrade to chitosan.The relative molecular mass of enzyme liberating method degradation process and degraded product is easy to be controlled, and directly carries out under relatively mild condition, and do not need to add other chemical reaction reagent, environmental pollution is few.But the enzymic degradation cycle is long, the easy inactivation of enzyme, production cost is high, is also difficult at present realize industrialization.
(3) physical degradation methods mainly radiation method, microwave method and supersonic method at present.Radiation degradation utilizes radioactive ray degrade chitosan, but radiation degradation is very high to equipment requirements, may produce hazardous and noxious substances simultaneously.Microwave method is degraded to chitosan by microwave radiation, but microwave degradation chitosan still rests on periodical operation at present, is difficult to continuous prodution.Ultrasonic degradation is mainly degraded to chitosan by ultrasound cavitation effect, its Degradation is fairly obvious, comparatively homogeneous low relative molecular mass chitosan can be obtained, and sonication acid amount obviously reduces, last handling process greatly simplifies, and also greatly reduces the pollution of environment.But due in total power consumption of ultrasonic cavitation, only have 5%-10% for cavitation effect, remaining 90%-95% makes system heat up with the form of heat energy.This intensification not only causes the waste of energy, is unfavorable for the process to heat-sensitive materials (industry such as biological example, medicine) simultaneously; Another serious problems of ultrasonic cavitation are its directivity and locality.Cavitation effect to only occur near ultra-sonic generator very in zonule, because bulk migration motion does not occur cavity, the formation of cavity, to develop and the process that crumbles and fall, just be limited in this limited area, thus, it is lower to there is capacity usage ratio in ultrasonic cavitation, the problems such as cavitation effect region is little, because sonication chitosan yield is too low, causes production cost too high, be difficult to industrial applications.
The applicant of the application is applying for not long ago and is obtaining the Chinese invention patent that the patent No. is ZL2010101787923, this patent utilizes equipment of Hydrodynamic Cavitation (Venturi tube) to prepare chitosan oligomer, but in follow-up R&D process, applicant finds: Hydrodynamic cavitation degraded is crumbled and fall by cavitation bubble and produce localized hyperthermia and high pressure around it, and with occurring strong shockwave and microjet, these physical conditions are that in solution, degradation of chitosan provides a favourable physicochemical environment, achieve and pass through free-radical oxidn, high temperature pyrolysis and supercritical water oxidation make chitosan molecule generation Degradation.But cavitation bubble is crumbled and fall rapidly, crumbles and fall after can not fully growing up again, and is difficult to the efficiency utilization realizing energy.
Summary of the invention
The technical problem to be solved in the present invention is: provide one to utilize self-vibration cavitation to prepare chitosan oligomer method, and the method is degraded to chitosan by the self-vibration cavitation effect of chitosan solution own, have simple and easy to do, energy consumption is low, efficiency high; There is the advantage of large-scale industrial application.
The technical scheme solved the problems of the technologies described above is: one utilizes self-vibration cavitation to prepare chitosan oligomer method, comprises the following steps:
The first step: chitosan dissolves: high molecular weight chitosan is added in solvent to dissolve and make chitosan solution, described solvent is the one among the buffered soln of inorganic acid aqueous solution, aqueous solutions of organic acids or slant acidity, wherein, described inorganic acid aqueous solution or the mass concentration of aqueous solutions of organic acids are 1%-13%, the pH of described buffered soln is 3-5, and the relative molecular mass of described high molecular weight chitosan is greater than 2 × 10
6, deacetylation is greater than 60%; Described mineral acid is hydrochloric acid, and organic acid is formic acid, acetic acid, lactic acid or citric acid, and described buffered soln is acetic acid-sodium acetate or citric acid-sodium citrate;
Second step: degraded;
3rd step: add alkaline solution in the chitosan solution after completing to degraded, adjustment pH is 9-10, precipitation, centrifugal throw out;
4th step: throw out acetone and washed with diethylether 1-3 time, namely vacuum-drying obtain chitosan oligomer;
The mass concentration of the chitosan solution described in the first step is 0.5g/L-5g/L;
Described second step is self-vibration cavitation technology: chitosan solution is carried out the process of self-vibration cavitation technology in self-vibration cavitation apparatus;
The pipeline that described self-vibration cavitation apparatus comprises water bath with thermostatic control cyclic water tank, basin, pump, self-vibration cavitation device and conveying chitosan solution and the tensimeter, the valve that are arranged on pipeline, described pump is communicated with basin, self-vibration cavitation device respectively by pipeline, and self-vibration cavitation device is communicated with basin by pipeline;
The technical process that described chitosan solution carries out self-vibration cavitation technology in self-vibration cavitation apparatus is: be placed on by chitosan solution in basin, and carry out constant temperature by cyclic water tank, chitosan solution carries out cavitation technology by pump delivery to self-vibration cavitation device, by valve regulated inlet pressure, and by tensimeter monitor force, the chitosan solution after self-vibration cavitation technology is back in basin;
The processing condition that chitosan solution carries out cavitation technology in self-vibration cavitation apparatus are:
inlet pressure: 0.1-0.6MPa;
temperature: 30-70 DEG C;
pH：3-5；
strength of solution: 0.5-5g/L;
degradation time: 0.5-10h, determines according to requiring the difference of product average molecular mass.
Described self-vibration cavitation device is the tubular structure with hollow space, along the flow direction of material, the hollow space of self-vibration cavitation device is respectively the first circular hole portion, the second circular hole portion, the 3rd circular hole portion, oared segrne pii and the 4th circular hole portion, the ratio of described first circular hole portion diameter D1 and the second circular hole portion D2 is the ratio of the 1.5 ~ 3.5, second circular hole portion D2 and the 3rd circular hole portion D3 is 1.5 ~ 5.
A kind of beneficial effect utilizing self-vibration cavitation to prepare chitosan oligomer method of the present invention is: the inventive method is dissolved the self-vibration cavitation effect of the chitosan solution made own and carried out degraded to high molecular weight chitosan by being added in solvent by high molecular weight chitosan and prepare chitosan oligomer, have simple and easy to do, energy consumption is low, efficiency high; Be significantly improved compared with the degradation rate that degradation rate of the present invention and existing equipment of Hydrodynamic Cavitation (Venturi tube) prepare chitosan oligomer, at least improve more than 40%, there is the advantage of large-scale industrial application.
Its principle is as follows: the generation of self-vibration cavitation be with a length be L, diameter be the organ tubular type resonator cavity of D2 as monofier, resonator cavity entrance and diameter are that the incoming flow pipe of D1 is connected, (D1/D2)
2form the entrance vena contracta of resonator cavity.Bottom and the diameter of resonator cavity are that the Outlet Section of D3 is connected, (D2/D3)
2form the exit constriction section of resonator cavity.Exit constriction section is autoexcitation mechanism, is again feedback mechanism.When stabilized fluid passes through, it is exciting that its contraction front can make fluid produce original pressure, pressure excitement can be fed back to resonator cavity again, forms feedback pressure vibration.Theoretical according to transient state stream, if the frequency of pressure excitement is mated with the natural frequency of resonator cavity, the pressure oscillation of feedback can be amplified, thus fluid resonant is produced in resonator cavity, form standing wave, in jet shear layer, eddy current becomes macrostructure separating cyclic eddy current, and the cavitation bubble that cavatition produces can be grown up in such a case fully, the energy produced when crumbling and fall is higher, thus effectively strengthens cavatition.And the shearing action of jet also contributes to the degraded of chitosan, the Hydrodynamic cavitation of efficiency ratio has greatly improved.
Accompanying drawing explanation
Fig. 1: the self-vibration cavitation apparatus structural representation of the present invention.
Fig. 2: the self-vibration cavitation device structural representation of the present invention.
In figure: 1-basin, 2-pump, 3-tensimeter, 4-self-vibration cavitation device, 41-first circular hole portion, 42-second circular hole portion, 43-the 3rd circular hole portion, 44-oared segrne pii, 45-the 4th circular hole portion, 5-water bath with thermostatic control cyclic water tank, 6-valve.
Embodiment
Embodiment: one utilizes self-vibration cavitation to prepare chitosan oligomer method, comprises the following steps:
The first step: chitosan dissolves: high molecular weight chitosan is added in solvent to dissolve and make chitosan solution, described solvent is the one among the buffered soln of inorganic acid aqueous solution, aqueous solutions of organic acids or slant acidity, wherein, described inorganic acid aqueous solution or the mass concentration of aqueous solutions of organic acids are 1%-13%, the pH of described buffered soln is 3-5, the mass concentration of described chitosan solution is 0.5g/L-5g/L, and the relative molecular mass of described high molecular weight chitosan is greater than 2 × 10
6, deacetylation is greater than 60%; Described mineral acid is hydrochloric acid, and organic acid is formic acid, acetic acid, lactic acid or citric acid, and described buffered soln is acetic acid-sodium acetate or citric acid-sodium citrate;
Second step: self-vibration cavitation technology: chitosan solution is carried out the process of self-vibration cavitation technology in self-vibration cavitation apparatus;
3rd step: add alkaline solution in the chitosan solution after completing to degraded, adjustment pH is 9-10, precipitation, centrifugal throw out;
4th step: throw out acetone and washed with diethylether 1-3 time, namely vacuum-drying obtain chitosan oligomer;
The pipeline that described self-vibration cavitation apparatus (as shown in Figure 1) comprises water bath with thermostatic control cyclic water tank 5, basin 1, pump 2, self-vibration cavitation device 4 and conveying chitosan solution and the tensimeter 3, the valve 6 that are arranged on pipeline, described pump is communicated with basin 1, self-vibration cavitation device 4 respectively by pipeline, and self-vibration cavitation device is communicated with basin by pipeline;
The technical process that described chitosan solution carries out self-vibration cavitation technology in self-vibration cavitation apparatus is: be placed on by chitosan solution in basin, and carry out constant temperature by cyclic water tank, chitosan solution carries out cavitation technology by pump delivery to self-vibration cavitation device, by valve regulated inlet pressure, and by tensimeter monitor force, the chitosan solution after self-vibration cavitation technology is back in basin;
The processing condition that chitosan solution carries out cavitation technology in self-vibration cavitation apparatus are:
inlet pressure: 0.1-0.6MPa;
temperature: 30-70 DEG C;
pH：3-5；
strength of solution: 0.5-5g/L;
degradation time: 0.5-10h, according to the different requirements to product average molecular mass, generally, require to be 20,000 when relative molecular mass, degradation time is 5-10h, and require to be 100,000 when relative molecular mass, degradation time is 1h.
In the present embodiment, described self-vibration cavitation device 4(is as shown in Figure 2) be the tubular structure with hollow space, along the flow direction of material, the hollow space of self-vibration cavitation device is respectively the first circular hole portion 41, second circular hole portion 42, the 3rd circular hole portion 43, oared segrne pii 44 and the 4th circular hole portion 45, the ratio of described first circular hole portion diameter D1 and the second circular hole portion D2 is 1.5 ~ 3.5, preferred value is the ratio of the 2.2, second circular hole portion D2 and the 3rd circular hole portion D3 is 1.5 ~ 5, and preferred value is 3.
Subordinate list 1: several concrete size of self-vibration cavitation device of the present invention.
Subordinate list 1 is only several embodiments of the concrete size of self-vibration cavitation device of the present invention, in actual application, can carry out suitable zooming in or out according to practical situation.
Subordinate list 2: a kind of relevant parameters table look-up utilizing self-vibration cavitation to prepare chitosan oligomer method of the present invention
Simultaneous test: adopt the method for the inventive method and Chinese patent ZL2010101787923 to do simultaneous test, the device used in the method for wherein Chinese patent ZL2010101787923 is Venturi tube, concrete processing parameter and experimental result as follows.
Simultaneous test 1: in degradation process, temperature 40 ° of C, pH4.4, pressure 0.4MPa, time 30min, chitosan solution concentration is different, and test-results is as subordinate list 3.
Subordinate list 3: simultaneous test 1 result.
Simultaneous test 2: in degradation process, chitosan solution concentration 3g/L, pH4.4, pressure 0.4MPa, time 30min, temperature is different, and test-results is as subordinate list 4.
Subordinate list 4: simultaneous test 2 result.
Simultaneous test 3: in degradation process, chitosan solution concentration 3g/L, temperature 40 ° of C, pressure 0.4MPa, time 30min, pH are different, and test-results is as subordinate list 5.
Subordinate list 5: simultaneous test 3 result.
Simultaneous test 4: in degradation process, chitosan solution concentration 3g/L, temperature 40 ° of C, pH4.4, time 30min, pressure is different, and test-results is as subordinate list 6.
Subordinate list 6: simultaneous test 4 result.
Simultaneous test 5: in degradation process, chitosan solution concentration 3g/L, temperature 40 ° of C, pH4.4, pressure 0.4MPa, the time is different, and test-results is as subordinate list 7.
Subordinate list 7: simultaneous test 5 result.
As can be seen from the result of above-mentioned contrast experiment, at least more than 40% is improved compared with the degradation rate that degradation rate of the present invention and existing equipment of Hydrodynamic Cavitation (Venturi tube) prepare chitosan oligomer, most cases can improve more than 50%, has individual cases even can improve more than 100%.Visible, compared with the present invention prepares the method for chitosan oligomer with existing equipment of Hydrodynamic Cavitation (Venturi tube), efficiency obviously wants high a lot.
Claims (2)
1. utilize self-vibration cavitation to prepare a chitosan oligomer method, comprise the following steps:
The first step: chitosan dissolves: high molecular weight chitosan is added in solvent to dissolve and make chitosan solution, described solvent is the one among the buffered soln of inorganic acid aqueous solution, aqueous solutions of organic acids or slant acidity, wherein, described inorganic acid aqueous solution or the mass concentration of aqueous solutions of organic acids are 1%-13%, the pH of described buffered soln is 3-5, and the relative molecular mass of described high molecular weight chitosan is greater than 2 × 10
6, deacetylation is greater than 60%; Described mineral acid is hydrochloric acid, and organic acid is formic acid, acetic acid, lactic acid or citric acid, and described buffered soln is acetic acid-sodium acetate or citric acid-sodium citrate;
Second step: degraded;
3rd step: add alkaline solution in the chitosan solution after completing to degraded, adjustment pH is 9-10, precipitation, centrifugal throw out;
4th step: throw out acetone and washed with diethylether 1-3 time, namely vacuum-drying obtain chitosan oligomer;
It is characterized in that:
The mass concentration of the chitosan solution described in the first step is 0.5g/L-5g/L;
Described second step is self-vibration cavitation technology: chitosan solution is carried out the process of self-vibration cavitation technology in self-vibration cavitation apparatus;
The pipeline that described self-vibration cavitation apparatus comprises water bath with thermostatic control cyclic water tank (5), basin (1), pump (2), self-vibration cavitation device (4) and conveying chitosan solution and the tensimeter (3), the valve (6) that are arranged on pipeline, described pump is communicated with basin (1), self-vibration cavitation device (4) respectively by pipeline, and self-vibration cavitation device is communicated with basin by pipeline;
The technical process that described chitosan solution carries out self-vibration cavitation technology in self-vibration cavitation apparatus is: be placed on by chitosan solution in basin, and carry out constant temperature by cyclic water tank, chitosan solution carries out cavitation technology by pump delivery to self-vibration cavitation device, by valve regulated inlet pressure, and by tensimeter monitor force, the chitosan solution after self-vibration cavitation technology is back in basin;
The processing condition that chitosan solution carries out cavitation technology in self-vibration cavitation apparatus are:
inlet pressure: 0.1-0.6MPa;
temperature: 30-70 DEG C;
pH：3-5；
strength of solution: 0.5-5g/L;
degradation time: 0.5-10h, determines according to requiring the difference of product average molecular mass.
2. one according to claim 1 utilizes self-vibration cavitation to prepare chitosan oligomer method, it is characterized in that: described self-vibration cavitation device (4) is the tubular structure with hollow space, along the flow direction of material, the hollow space of self-vibration cavitation device is respectively the first circular hole portion (41), the second circular hole portion (42), the 3rd circular hole portion (43), oared segrne pii (44) and the 4th circular hole portion (45), the ratio of described first circular hole portion diameter D1 and the second circular hole portion D2 is the ratio of the 1.5 ~ 3.5, second circular hole portion D2 and the 3rd circular hole portion D3 is 1.5 ~ 5.
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Cited By (4)
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| CN108342514A (en) * | 2017-01-23 | 2018-07-31 | 广西科技大学 | The method of self-excited oscillation pulse cavitation reinforcement cane juice clarification |
| CN109964931A (en) * | 2019-03-27 | 2019-07-05 | 广西科技大学 | A kind of method that jet self-excited pulse cavitation reinforcement prepares the antibacterial nanosphere of chitosan |
| CN110841574A (en) * | 2019-11-19 | 2020-02-28 | 西安交通大学 | Hydrodynamic cavitation device for introducing crystal defects into nano material and operation method thereof |
| CN114455770A (en) * | 2022-03-01 | 2022-05-10 | 辽宁大学 | Method for treating dye wastewater and generating heat by heat-assisted reinforced hydrodynamic cavitation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342514A (en) * | 2017-01-23 | 2018-07-31 | 广西科技大学 | The method of self-excited oscillation pulse cavitation reinforcement cane juice clarification |
| CN109964931A (en) * | 2019-03-27 | 2019-07-05 | 广西科技大学 | A kind of method that jet self-excited pulse cavitation reinforcement prepares the antibacterial nanosphere of chitosan |
| CN109964931B (en) * | 2019-03-27 | 2021-07-20 | 广西科技大学 | Method for preparing chitosan antibacterial nano-microspheres by jet self-excitation pulse cavitation enhancement |
| CN110841574A (en) * | 2019-11-19 | 2020-02-28 | 西安交通大学 | Hydrodynamic cavitation device for introducing crystal defects into nano material and operation method thereof |
| CN114455770A (en) * | 2022-03-01 | 2022-05-10 | 辽宁大学 | Method for treating dye wastewater and generating heat by heat-assisted reinforced hydrodynamic cavitation |
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