CN1493577A - Technology and equipment for preparing chitin oligo saccharide - Google Patents
Technology and equipment for preparing chitin oligo saccharide Download PDFInfo
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- CN1493577A CN1493577A CNA021255288A CN02125528A CN1493577A CN 1493577 A CN1493577 A CN 1493577A CN A021255288 A CNA021255288 A CN A021255288A CN 02125528 A CN02125528 A CN 02125528A CN 1493577 A CN1493577 A CN 1493577A
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Abstract
A process and equipment for preparing chitoligose from chitosan feature that the microwave circulating fluidized-bed reactor is used and the hydrogen peroxide is used for oxidizing degradation to obtain chitoligose. Its advantages are high productivity increased by 10 times and controllable molecular weight of product.
Description
Technical field
The present invention relates to a kind of technology and equipment for preparing chitin oligo saccharide.
Background technology
Chitosan degraded preparation chitin oligo saccharide has several different methods, as oxidative degradation, acid degradation and enzyme liberating or the like.But don't work which kind of method, degradation time is all very long, generally needs 5-6 hour, even tens hours just can obtain needed oligosaccharides.Currently used equipment is traditional stirred reactor, long reaction time, and production intensity is low, at present also not about improving the report of degradation efficiency.
Micro-wave energy is accelerated the speed of chemical reaction, and circulating fluidized bed has been strengthened the contact between liquid-solid, thereby has accelerated speed of response.
Summary of the invention
The object of the present invention is to provide a kind of technology and equipment for preparing chitin oligo saccharide, adopt the microwave circulating fluid bed reactor to carry out the DeR of chitosan, can improve degradation efficiency greatly.
The present invention passes through following scheme implementation:
At first prepare the aqueous solution of different hydrogen peroxide weight percent concentration, add the chitosan powder again, fixedly chitosan solid weight percentage concentration pumps in the reactor with volume pump from charging opening, begins to feed microwave heating after whole bed is full of material, by the thermometer control reaction temperature.After circulation tube is full of material, suspend and feed in raw material, open recycle pump and carry out the circulating fluidization reaction.Chitin oligo saccharide after the degraded is water-soluble, is discharged by control valve through filter.Behind the mean residence time that reaches setting, continue the amount of using tricks pump quantifying feed, open the quantitative expel liquid of control valve, form successive reaction, add the discharge process continuously, in the process that continues operation, can change temperature of reaction, feed rate, solid-to-liquid ratio, concentration of hydrogen peroxide, with oligosaccharides and the maximum production efficiency that obtains different molecular weight; The liquid of discharging obtains the oligosaccharides product of different molecular weight by concentrate drying.
Process of the present invention does not have the waste water,waste gas and industrial residue discharging, belongs to the pollution-free chemical industry course of processing.Flow process of the present invention and traditional process compare, owing to accelerated speed of response, the production intensity of equipment has improved nearly 10 times, product oligosaccharide molecular amount narrow distribution, and the while can arbitrarily be controlled the molecular weight of different oligosaccharides products.
Description of drawings
Fig. 1: the circulating fluidized fluidized bed reactor structural representation of microwave.
Description of symbols:
(1) reactor (2) thermometer
(3) microwave cavity (4) blow-off valve
(5) recycle pump (6) control valve
(7) strainer (8) circulation tube
Specific embodiments
Below further specify the present invention with preferred embodiment.Among the following embodiment: reactor (1) diameter is 100mm, and height is 2000mm, and circulation tube (8) diameter is 20nn, and reactor (1) volume is 150L.
Embodiment 1:
Take by weighing the 10Kg chitosan and add the 890Kg pure water and be made into 900Kg solid suspension solution, get 30% hydrogen peroxide 100Kg again and add, stir, pump in the reactor (1) by charge pump from charging opening with the speed of 600kg per hour.After whole reactor (1) and circulation tube (8) all are full of solution, suspend reinforcedly, to microwave cavity (3) in, import microwave, start recycle pump (5) simultaneously and circulate with 1 cubic metre flow per hour.When thermometer (2) displays temperature was raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by pressure controlled valve (6) through filter (7).Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 6kg/h, average viscosity-average molecular weight 4500.
Embodiment 2:
Take by weighing the 40Kg chitosan and add the 860Kg pure water and be made into 900Kg solid suspension solution, get 30% hydrogen peroxide 100Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 12kg/h, average viscosity-average molecular weight 3400.
Embodiment 3:
Take by weighing the 60Kg chitosan and add the 840Kg pure water and be made into 900Kg solid suspension solution, get 30% hydrogen peroxide 100Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 13.5kg/h, average viscosity-average molecular weight 2700.
Embodiment 4:
Take by weighing the 100Kg chitosan and add the 800Kg pure water and be made into 900Kg solid suspension solution, get 30% hydrogen peroxide 100Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 15kg/h, average viscosity-average molecular weight 1600.
Embodiment 5:
Take by weighing the 50Kg chitosan and add the 933.33Kg pure water and be made into 983.33Kg solid suspension solution, get 30% hydrogen peroxide 16.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 7.5kg/h, average viscosity-average molecular weight 5000.
Embodiment 6:
Take by weighing the 50Kg chitosan and add the 883.33Kg pure water and be made into 933.33Kg solid suspension solution, get 30% hydrogen peroxide 66.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 11.3kg/h, average viscosity-average molecular weight 3500.
Embodiment 7:
Take by weighing the 50Kg chitosan and add the 850Kg pure water and be made into 900Kg solid suspension solution, get 30% hydrogen peroxide 100Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 12.8kg/h, average viscosity-average molecular weight 2700.
Embodiment 8:
Take by weighing the 50Kg chitosan and add the 783.33Kg pure water and be made into 833.33Kg solid suspension solution, get 30% hydrogen peroxide 166.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 70 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 15kg/h, average viscosity-average molecular weight 1000.
Embodiment 9:
Take by weighing the 50Kg chitosan and add the 883.33Kg pure water and be made into 933.33Kg solid suspension solution, get 30% hydrogen peroxide 66.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 40 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 7.5kg/h, average viscosity-average molecular weight 4600.
Embodiment 10:
Take by weighing the 50Kg chitosan and add the 883.33Kg pure water and be made into 933.33Kg solid suspension solution, get 30% hydrogen peroxide 66.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 60 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 10kg/h, average viscosity-average molecular weight 3300.
Embodiment 11:
Take by weighing the 50Kg chitosan and add the 883.33Kg pure water and be made into 933.33Kg solid suspension solution, get 30% hydrogen peroxide 66.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 75 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 12.8kg/h, average viscosity-average molecular weight 2000.
Embodiment 12:
Take by weighing the 50Kg chitosan and add the 883.33Kg pure water and be made into 933.33Kg solid suspension solution, get 20% hydrogen peroxide 66.67Kg again and add, stir, pump in the reactor by charge pump from charging opening with the speed of 600kg per hour.After whole reactor and circulation tube all are full of solution, suspend reinforcedly, in microwave cavity, import microwave, start recycle pump simultaneously and circulate with 1 cubic metre flow per hour.When treating that temperature is raised to 90 ℃, it is temperature-resistant that temperature controlling system will keep, and at this moment reopens charge pump, and with the per hour feed rate adding of 600kg, the solution after the degraded is discharged by the pressure-controlling blow-off valve through filter.Carry out the operation of successive temperature attitude, get one time sample every half an hour, 6 samples are got in continuous temperature attitude operation 3 hours.Weigh behind the concentrate drying respectively, measure viscosity-average molecular weight, get the viscosity-average molecular weight of the mean value of these 6 samples as this condition.Consequently productive rate is 22.5kg/h, average viscosity-average molecular weight 600.
Claims (6)
1, a kind of technology for preparing chitin oligo saccharide is characterized in that: be raw material with the chitosan, adopt the circulating fluidized fluidized bed reactor of microwave, with the hydrogen peroxide preparation chitin oligo saccharide of degrading continuously; In reaction process, the weight percent concentration of regulating chitosan is 1%-10%, and the weight percent concentration of hydrogen peroxide is 0.5%-5.0%, and temperature of reaction is 40-90 ℃.
2, the technology of the described preparation chitin oligo saccharide of claim 1 is characterized in that: in reaction process, the weight percent concentration of regulating chitosan is 3%-6%.
3, the technology of the described preparation chitin oligo saccharide of claim 1 is characterized in that: in reaction process, the weight percent concentration of hydrogen peroxide is 2%-3%.
4, the technology of the described preparation chitin oligo saccharide of claim 2 is characterized in that: in reaction process, the weight percent concentration of hydrogen peroxide is 2%-3%.
5, the technology of each described preparation chitin oligo saccharide of claim 1-4 is characterized in that: temperature of reaction is 65-75 ℃.
6, a kind of equipment as each described preparation chitin oligo saccharide technology of claim 1 to 4, it is characterized in that, this equipment is the circulating fluidized fluidized bed reactor of microwave, and it comprises: circulation bed, circulation tube, microwave cavity, recycle pump, thermometer, reinforced and discharge device.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02125528 CN1219783C (en) | 2002-07-18 | 2002-07-18 | Technology and equipment for preparing chitin oligo saccharide |
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| CN 02125528 CN1219783C (en) | 2002-07-18 | 2002-07-18 | Technology and equipment for preparing chitin oligo saccharide |
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| CN1493577A true CN1493577A (en) | 2004-05-05 |
| CN1219783C CN1219783C (en) | 2005-09-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2213678A1 (en) * | 2007-10-17 | 2010-08-04 | Nippon Steel Chemical Co., Ltd. | Production methods for solubilized lignin, saccharide raw material and monosaccharide raw material, and solubilized lignin |
| CN102702386A (en) * | 2012-06-14 | 2012-10-03 | 中国科学院海洋研究所 | Method for degrading chitosan |
| DE102012009593A1 (en) | 2012-05-07 | 2013-11-07 | Innovent E.V. | Degradation of polysaccharides, comprises reacting solutions or suspensions of polysaccharide with chlorine dioxide, in which degree of chain degradation is controlled by concentrating chlorine dioxide and polysaccharide |
| CN104072634A (en) * | 2014-07-16 | 2014-10-01 | 中国科学院海洋研究所 | Preparation method for chitin oligosaccharides |
-
2002
- 2002-07-18 CN CN 02125528 patent/CN1219783C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2213678A1 (en) * | 2007-10-17 | 2010-08-04 | Nippon Steel Chemical Co., Ltd. | Production methods for solubilized lignin, saccharide raw material and monosaccharide raw material, and solubilized lignin |
| CN101848920A (en) * | 2007-10-17 | 2010-09-29 | 新日铁化学株式会社 | Production methods for solubilized lignin, saccharide raw material and monosaccharide raw material, and solubilized lignin |
| EP2213678A4 (en) * | 2007-10-17 | 2012-05-02 | Nippon Steel Chemical Co | Production methods for solubilized lignin, saccharide raw material and monosaccharide raw material, and solubilized lignin |
| US9133227B2 (en) | 2007-10-17 | 2015-09-15 | Nippon Steel & Sumikin Chemical Co., Ltd. | Production methods for solubilized lignin, saccharide raw material and monosaccharide raw material, and solubilized lignin |
| DE102012009593A1 (en) | 2012-05-07 | 2013-11-07 | Innovent E.V. | Degradation of polysaccharides, comprises reacting solutions or suspensions of polysaccharide with chlorine dioxide, in which degree of chain degradation is controlled by concentrating chlorine dioxide and polysaccharide |
| DE102012009593B4 (en) | 2012-05-07 | 2019-03-07 | Innovent E.V. | Process for the degradation of polysaccharides selected from the substance groups of the glycosaminoglycans and their derivatives and the alginates |
| CN102702386A (en) * | 2012-06-14 | 2012-10-03 | 中国科学院海洋研究所 | Method for degrading chitosan |
| CN104072634A (en) * | 2014-07-16 | 2014-10-01 | 中国科学院海洋研究所 | Preparation method for chitin oligosaccharides |
| CN104072634B (en) * | 2014-07-16 | 2016-10-05 | 中国科学院海洋研究所 | A kind of chitin oligose preparing process |
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| CN1219783C (en) | 2005-09-21 |
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