CN102021252B - Method and device for continuously hydrolyzing corn bran - Google Patents
Method and device for continuously hydrolyzing corn bran Download PDFInfo
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- CN102021252B CN102021252B CN 201010598948 CN201010598948A CN102021252B CN 102021252 B CN102021252 B CN 102021252B CN 201010598948 CN201010598948 CN 201010598948 CN 201010598948 A CN201010598948 A CN 201010598948A CN 102021252 B CN102021252 B CN 102021252B
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Abstract
The invention relates to a method and device for continuously hydrolyzing corn brans, belonging to the technical field of corn deep processing. The method comprises the following steps: (1) mixing the corn brans with hydrolytic acid, and pre-leaching for 5-10 minutes; (2) heating the material mixed and pre-leached in the step (1) to 115-125 DEG C, and hydrolyzing for 2.5-3.5 hours to obtain hydrolyzate; (3) cooling the hydrolyzate prepared in the step (2), and then separating the hydrolyzate from residues; and (4) when the component content in the hydrolyzate separated in the step (3) meets the requirement, exporting the hydrolyzate separated in the step (3), and carrying out sugar separation; when the component content in the hydrolyzate separated in the step (3) is lower than the required content, leading the hydrolyzate to enter the step (1) to mix with the corn brans, pre-leaching for 5-10 minutes, and recycling. By the method and equipment in the invention, the continuous hydrolysis of the corn brans is achieved, the yield equipment with the same scale has the advantages of low investment, high production efficiency and low energy consumption and is convenient for automatic operation, and the quality of the hydrolyzate is stable.
Description
Technical field
The present invention relates to a kind of continuous hydrolysis corn husk method and apparatus, belong to the corn deep processing technology field.
Background technology
Maize peel is the by product of production of corn starch, and its output generally reaches 12.5% of corn total amount, and the value of product is lower, sells mainly as feedstuff raw material.Maize peel contains abundant Mierocrystalline cellulose and hemicellulose, can obtain various carbohydrates take acid as catalyzer after the hydrolysis, comprises hexose and five-carbon sugar, wood sugar 30-35% wherein, the about 20-23% of pectinose, therefore glucose 20-26% can be used as the raw material of producing wood sugar and pectinose.
Wood sugar is extraordinary functional food additives, and after particularly further hydrogenation became Xylitol, purposes was more extensive.Pectinose is the same with wood sugar, all belongs to five-carbon sugar, and the sweet taste of similar sucrose is arranged, and pectinose is important medicine intermediate, can be used to the medicine of synthetic anticancer, antiviral and Cardiovarscular.Compare with wood sugar, the physiological function that has as the pectinose of five-carbon sugar is more peculiar.In recent years international physiologist and nutritionist with regard to pectinose in enteron aisle to a series of further investigations of being used as of sugar metabolism, find that pectinose has remarkable blocking effect to the metabolic conversion of sucrose, so that it is good in the application prospect of the aspects such as fat-reducing, control diabetes.Produce at present wood sugar, Xylitol take corn cob as raw material, adopt the interrupter method hydrolysis, and then refining forming, but since the corn cob supply seasonal strong, and be difficult to store, corn cob in short supply restricted further developing of wood sugar, Xylitol enterprise.And maize peel is in liberal supply concerning corn deep processing enterprise, stable, particularly the content of pectinose is much higher than other raw materials after the maize peel hydrolysis, being the best raw material of producing pectinose, is the developing direction of from now on maize peel deep processing as raw material production wood sugar and pectinose take maize peel therefore.
Method for hydrolysis and technique are one of gordian techniquies take maize peel as raw material production wood sugar and pectinose, and hydrolysis process is directly connected to the yield of wood sugar and pectinose, and method for hydrolysis and device directly have influence on large production cost.The reactor intermittent hydrolysis is all adopted at present China's corn cob hydrolysis, and production efficiency is low, energy consumption is high, and quality is unstable, is not easy to automatization, stream line operation.The research of maize peel hydrolysis is just at the early-stage, also be to adopt batch technology and equipment, therefore the realization of continuous hydrolysis corn husk technique and device, can improve hydrolysis production efficiency, reduce energy consumption, improve the hydrolyzed solution quality, can realize and the screenings separation circuit operate continuously of rear road simultaneously, to China take maize peel as the raw material production wood sugar and pectinose have great importance, to corn cob method for hydrolysis and equipment important reference being arranged also.
Publication number is the Chinese patent application of CN 101824055A, and disclosing a kind of maize peel is the method that raw material prepares L-arabinose, belongs to technical field of functional sugar.It comprises: boiling: the raw material maize peel is added the alkali lye boiling; Acid treatment: with the maize peel of oxalic acid treatment boiling, collect hydrolyzed solution; Neutralization: add calcium carbonate aqueous solution, neutralization, insulation, suction filtration, neutralizer.Decolouring: with the neutralizer activated carbon decolorizing, get destainer; Desalination removal of impurities: destainer through positively charged ion and anionite-exchange resin desalination removal of impurities, is once exchanged liquid; Concentrating under reduced pressure: will once exchange the liquid concentrating under reduced pressure, and get single vaporization liquid; Secondary decolourization: suction filtration after the decolouring gets secondary decolourization liquid.Secondary desalination: secondary decolourization liquid through positively charged ion and anionite-exchange resin secondary desalination removal of impurities, is obtained secondary exchange liquid; Chromatographic separation: secondary is exchanged the liquid evaporation concentration, carry out chromatographic separation; Exchange liquid concentrating under reduced pressure with after the chromatographic separation is cooled to room temperature naturally; Centrifugal oven dry: centrifugal, oven dry gets the crystal pectinose.This technique is hydrolyzed by acid treatment by after first material being heated up again, and obtains hydrolyzed solution, belongs to intermittent hydrolysis technique, and not only energy consumption height, and hydrolyzed solution quality and production efficiency are all lower.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of continuous hydrolysis corn husk method and apparatus is provided.
A kind of continuous hydrolysis corn husk method may further comprise the steps:
(1) maize peel and hydrolysis acid are mixed, preimpregnation 5-10min;
(2) step (1) is mixed, the heating material after the preimpregnation after 115-125 ℃, hydrolysis 2.5-3.5h gets hydrolyzed solution;
(3) after the hydrolyzed solution cooling that step (2) is made, separate hydrolyzed solution and material slag;
(4) when component content meets the requirements in the isolated hydrolyzed solution of step (3), hydrolyzed solution is derived, carry out sugar from operation, when component content is lower than requirement in the isolated hydrolyzed solution of step (3), hydrolyzed solution enters step (1), mix with maize peel, preimpregnation 5-10min, carry out cyclical operation.
Described hydrolysis acid is the sulfuric acid of 1.2-1.8% for concentration, and addition is the hydrolysis acid that the per unit weight maize peel adds the 8-10 unit weight.
Preferably, sulfuric acid concentration is 1.5%, and addition is the hydrolysis acid that the per unit weight maize peel adds 9 unit weights.
Heating material mode in the described step (2) is the injection instantaneously heating take steam as thermal source.
Hydrolysis temperature in the described step (2) is 118 ℃, and hydrolysis time is 3h.
The mode of the hydrolyzed solution cooling in the described step (3) adopts the flash distillation cooling; The mode of separating hydrolyzed solution and material slag adopts the expeller expression separation.
The specific equipment of above-mentioned continuous hydrolysis corn husk method, comprise the material feedway, mixing device, heating unit, hydrolysis reactor, heat sink, the screenings tripping device, it is characterized in that, the material feedway is connected with the opening for feed of mixing device, the discharge port of mixing device is connected with the opening for feed of heating unit, the discharge port of heating unit is connected with the opening for feed of hydrolysis reactor, the discharge port of hydrolysis reactor is connected with the opening for feed of heat sink, the discharge port of heat sink is connected with the opening for feed of screenings tripping device, and the grout outlet of screenings tripping device is connected with the opening for feed of outlet pipe and mixing device respectively.
Described material feedway comprises sulphuric acid soln storage tank, under meter, belt feeder, impact type flow of bulk-solid meter, the sulphuric acid soln storage tank is connected by pipeline with the liquid inlet opening of impact type flow of bulk-solid meter, be provided with under meter on the pipeline, the discharge port of belt feeder is connected with the solid materials opening for feed of impact type flow of bulk-solid meter, and the discharge port of impact type flow of bulk-solid meter is connected with the opening for feed of mixing device;
Described mixing device is the thread mixing Presoaker.Be provided with the uniform pitch screw propulsion rod in this device, can satisfy mixing of materials preimpregnation time 5-10 minute requirement.
Described heating unit comprises surge tank, nothing obstruction screenings pump, vacuum breaker, injector, thermometer, surge tank stops up the screenings pump with nothing and is connected by pipeline, be provided with vacuum breaker on the pipeline, be connected with injector by pipeline without stopping up the screenings pump, be provided with thermometer on the injector.Injector adopts the graduate HYZ type of Shanghai million light series high voltage steam injector.
Described screenings tripping device comprises screw squeezer, hydrolyzed solution surge tank, acid proof pump, valve and under meter, the liquid discharge port of screw squeezer is communicated with hydrolyzed solution surge tank opening for feed, hydrolyzed solution surge tank discharge port be connected by pipeline with the opening for feed of outlet pipe and mixing device respectively, be provided with acid proof pump, valve and under meter on this pipeline.Screw squeezer separates for the screenings of the material that is hydrolyzed, and the screw propulsion rod of varying pitch is housed in the screw squeezer.
Tensimeter and thermometer are arranged on the described hydrolysis reactor, this hydrolysis reactor has pot type and 2 kinds of structure formations of tubular type, adopt the tank reactor tank diameter at 0.5-1.5m, adopt the tangential feeding mode of low in and high out, make the material that is introduced into reactor first out, all reach requirement to guarantee the reaction times.The tank body quantity (length of pipeline) that reactor is included and volume energy satisfy and got final product in reaction times 2.5-3.5 hour.
Described heat sink is flash tank, and its top is divided into right cylinder, and the bottom is cone, takes the mode of tangential feeding on cylinder top; This feeding manner can prolong evaporation time and increase evaporation area.
The contact surface of contact acid solution or acid materials device is all selected Stainless steel 316 L in aforesaid device, or carries out enamel anticorrosion and process.
Continuous hydrolysis corn husk method and apparatus provided by the invention also is applicable to the biomass materials such as corn cob, bagasse, stalk through pulverizing except being applicable to maize peel, to different materials, hydrolysis process needs suitably to adjust.
The present invention compared with prior art has the following advantages:
1, realized the serialization of maize peel hydrolysis, the output facility investment of same size is few, and production efficiency is high, and energy consumption is low.
2, be convenient to automated operation, reduce labour intensity, the hydrolyzed solution quality is more stable simultaneously.
3, adopted the mode of vapo(u)r blasting heating, realized instantaneously heating to hydrolysis temperature, efficient is high, and is energy-conservation.
4, separate the backflow of rear hydrolyzed solution by screenings, realize the again circulation hydrolysis of hydrolyzed solution, improve the concentration of hydrolyzed solution, greatly reduce follow-up refining and evaporation expense, compare with the intermittent hydrolysis method and apparatus, reduced facility investment, production efficiency improves greatly, be conducive to simultaneously the linking with later process, realize producing continuously, for having laid good basis take maize peel as the industrializing implementation of raw material production wood sugar and pectinose.
Description of drawings
Fig. 1 is continuous hydrolysis corn husk device synoptic diagram;
Wherein: 1, acid solution storage tank, 2, valve, 3, under meter, 4, belt feeder, 5, impact type flow of bulk-solid meter, 6, the thread mixing Presoaker, 7, surge tank, 8, without stopping up the screenings pump, 9, vacuum breaker, 10, magnetic flow meter, 11, injector, 12, thermometer, 13, tensimeter, 14, hydrolysis reactor, 15, flash tank, 16, screw squeezer, 17, the hydrolyzed solution surge tank, 18, acid proof pump.
Embodiment
The present invention will be further described below in conjunction with Figure of description and embodiment.
Embodiment 1
A kind of continuous hydrolysis corn husk method may further comprise the steps:
(1) be that 1.5% sulfuric acid mixes, preimpregnation 10min with maize peel and concentration, the sulfuric acid addition is the sulfuric acid that the per unit weight maize peel adds 9 unit weights;
(2) step (1) is mixed, to adopt steam be that hydrolysis 3h got hydrolyzed solution after the injection instantaneously heating mode of thermal source was heated to 118 ℃ to the material after the preimpregnation;
(3) hydrolyzed solution that step (2) is made adopts the flash distillation cooling method to be down to 80-85 ℃, adopts expeller expression separation hydrolyzed solution and material slag;
After testing, hydrolyzed solution solid content 9.3%, main component is as follows:
Hydrochlorate 31.24%, glucose 19.53%, wood sugar 29.62%, pectinose 16.32%, surplus impurity.
Hydrolyzed solution and the maize peel that embodiment 1 is made mixed by weight 1: 9, preimpregnation 10min, repeated the operation of embodiment 1 step (2) and step (3).
After testing, hydrolyzed solution solid substance thing content 17.1%, main component is as follows:
Hydrochlorate 25.03%, glucose 20.92%, wood sugar 31.79%, pectinose 19.96%, surplus impurity.
After the circulation hydrolysis, solid content improves nearly one times, and the ratio of sugar component is substantially constant, has saved consumption and the energy consumption of sulfuric acid.
Embodiment 3
The specific equipment of above-mentioned continuous hydrolysis corn husk method, as shown in Figure 1, comprise the material feedway, mixing device, heating unit, hydrolysis reactor, heat sink, the screenings tripping device, the material feedway is connected with the opening for feed of mixing device, the discharge port of mixing device is connected with the opening for feed of heating unit, the discharge port of heating unit is connected with the opening for feed of hydrolysis reactor, the discharge port of hydrolysis reactor is connected with the opening for feed of heat sink, the discharge port of heat sink is connected with the opening for feed of screenings tripping device, and the grout outlet of screenings tripping device is connected with the opening for feed of outlet pipe and mixing device respectively.
Above-mentioned material feedway comprises acid solution storage tank 1, under meter 3, belt feeder 4, impact type flow of bulk-solid meter 5, acid solution storage tank 1 is connected by pipeline with the liquid inlet opening of impact type flow of bulk-solid meter 5, be provided with under meter 3 on the pipeline, the discharge port of belt feeder 4 is connected with the solid materials opening for feed of impact type flow of bulk-solid meter 5, and the discharge port of impact type flow of bulk-solid meter 5 is connected with the opening for feed of mixing device;
Above-mentioned mixing device is thread mixing Presoaker 6.Be provided with the uniform pitch screw propulsion rod in this device, can satisfy mixing of materials preimpregnation time 5-10 minute requirement.
Above-mentioned heating unit comprises surge tank 7, nothing obstruction screenings pump 8, vacuum breaker 9, injector 11, thermometer 12, surge tank 7 be connected by pipeline without stopping up screenings pump 8, be provided with vacuum breaker 9 on the pipeline, be connected with injector 11 by pipeline without stopping up screenings pump 8, be provided with thermometer 12 on the injector 11.Injector 11 is HZY-5 type injectors that Shanghai million smooth research institute company limiteds produce.
Above-mentioned screenings tripping device comprises screw squeezer 16, hydrolyzed solution surge tank 17, acid proof pump 18, valve 2 and under meter 3, the liquid discharge port of screw squeezer 16 is communicated with hydrolyzed solution surge tank 17 opening for feeds, hydrolyzed solution surge tank 17 discharge ports be connected by pipeline with the opening for feed of outlet pipe and mixing device respectively, be provided with acid proof pump 18, valve 5 and under meter 3 on this pipeline.Screw squeezer 16 separates for the screenings of the material that is hydrolyzed, and the screw propulsion rod of varying pitch is housed in the screw squeezer 16.
Tensimeter 13 and thermometer 12 are arranged on the said hydrolyzed reactor 14, this hydrolysis reactor adopts the tank reactor tank diameter at 1m, adopt the tangential feeding mode of low in and high out, make the material that is introduced into hydrolysis reactor 14 first out, all reach requirement to guarantee the reaction times.Hydrolysis reactor 14 comprises 4 tank bodies, and the reaction times reaches 2.5-3.5 hour.
Above-mentioned heat sink is flash tank 15, and its top is divided into right cylinder, and the bottom is cone, takes the mode of tangential feeding on cylinder top; This feeding manner can prolong evaporation time and increase evaporation area.
The acidproof magnetic flow meter of the preferential employing of under meter in the present embodiment is with transmission and the automatically control that makes things convenient for signal; The belt feeder motor adopts variable frequency control, with convenient control material addition.The contact surface material selection Stainless steel 316 L of the equipment of all contact acid solutions or acid material.
Take dried maize peel material as example, maize peel enters Flow Meter for Solid Materials 5 by belt feeder 4 and carries out flow metering, rotating speed by the control belt feeder carries out flow control, the 1.2-1.8% sulphuric acid soln of acid solution storage tank 1 the inside enters the thread mixing Presoaker simultaneously by valve 2 and under meter 3 with from Flow Meter for Solid Materials 5 maize peel out, by the flow of liquor ratio control in 1: 8 maize peel and acid solution, mix preimpregnation time maintenance 10min.
Material after the preimpregnation enters surge tank 7, then by squeezing into injector 11 without stopping up screenings pump 8, realize under the vapor action that enters at the same time that instantaneously heating is to hydrolysis temperature 115-125 ℃, steam is controlled by valve 2, feeding pipe at injector is equipped with vacuum breaker 9, there be simultaneously valve 2 and under meter 10 to realize flow control and meterings, be provided with thermometer 12 at the lower part outlet of injector, carry out temperature survey.
Enter hydrolysis reactor 14 reactions 3.5 hours from injector bottom material out from bottom tangent.Hydrolysis reactor 14 is comprised of 4 tank bodies, and the valve 2 that is equipped with tensimeter 13, thermometer 12 and keeps pressure, enter flash tank 15 after hydrolysis is finished and carry out the flash distillation cooling, then adopting screw squeezer 16 to carry out screenings separates, hydrolyzed solution enters hydrolyzed solution surge tank 17, the mixing Presoaker of being squeezed into next procedure or being back to leading portion by acid proof pump 18 hydrolysis that circulates improving hydrolyzed solution concentration, is equipped with valve 2 and under meter 3 is used for flow control and metering at the discharging pipeline of pump.
Continuous hydrolysis corn husk method and apparatus provided by the invention is except being applicable to maize peel, also be applicable to the biomass materials such as corn cob, bagasse, stalk through pulverizing, to different materials, the hydrolysis process parameter needs suitably to adjust, to reach best hydrolysis effect.
More than describing in detail is that this embodiment limits claim of the present invention for the specifying of possible embodiments of the present invention, and the equivalence that all the present invention of disengaging do is implemented or change, all should be contained in the claim of the present invention.
Claims (7)
1. a continuous hydrolysis corn husk method is characterized in that, is comprised of following steps:
(1) maize peel and hydrolysis acid are mixed, preimpregnation 5-10min;
(2) step (1) is mixed, the heating material after the preimpregnation after 115-125 ℃, hydrolysis 2.5-3.5h gets hydrolyzed solution;
(3) after the hydrolyzed solution cooling that step (2) is made, separate hydrolyzed solution and material slag;
(4) when component content meets the requirements in the isolated hydrolyzed solution of step (3), hydrolyzed solution is derived, carry out sugar from operation, when component content is lower than requirement in the isolated hydrolyzed solution of step (3), hydrolyzed solution enters step (1), mix with maize peel, preimpregnation 5-10min, carry out cyclical operation;
Hydrolysis acid in the described step (1) is the sulfuric acid of 1.2-1.8% for concentration, and addition is the hydrolysis acid that the per unit weight maize peel adds the 8-10 unit weight;
Heating material mode in the described step (2) is the injection instantaneously heating take steam as thermal source;
The mode of the hydrolyzed solution cooling in the described step (3) adopts the flash distillation cooling; The mode of separating hydrolyzed solution and material slag adopts the expeller expression separation.
2. method for hydrolysis as claimed in claim 1 is characterized in that, sulfuric acid concentration is 1.5%, and addition is the hydrolysis acid that the per unit weight maize peel adds 9 unit weights.
3. method for hydrolysis as claimed in claim 1 is characterized in that, the hydrolysis temperature in the described step (2) is 118 ℃, and hydrolysis time is 3h.
4. the specific equipment of the described continuous hydrolysis corn husk method of claim 1, comprise the material feedway, mixing device, heating unit, hydrolysis reactor, heat sink, the screenings tripping device, it is characterized in that, the material feedway is connected with the opening for feed of mixing device, the discharge port of mixing device is connected with the opening for feed of heating unit, the discharge port of heating unit is connected with the opening for feed of hydrolysis reactor, the discharge port of hydrolysis reactor is connected with the opening for feed of heat sink, the discharge port of heat sink is connected with the opening for feed of screenings tripping device, and the grout outlet of screenings tripping device is connected with the opening for feed of outlet pipe and mixing device respectively;
Described heating unit comprises surge tank, nothing obstruction screenings pump, vacuum breaker, injector, thermometer, surge tank stops up the screenings pump with nothing and is connected by pipeline, be provided with vacuum breaker on the pipeline, be connected with injector by pipeline without stopping up the screenings pump, be provided with thermometer on the injector.
5. described specific equipment as claimed in claim 4, it is characterized in that, the material feedway comprises sulphuric acid soln storage tank, under meter, belt feeder, impact type flow of bulk-solid meter, the sulphuric acid soln storage tank is connected by pipeline with the liquid inlet opening of impact type flow of bulk-solid meter, be provided with under meter on the pipeline, the discharge port of belt feeder is connected with the solid materials opening for feed of impact type flow of bulk-solid meter, and the discharge port of impact type flow of bulk-solid meter is connected with the opening for feed of mixing device.
6. described specific equipment as claimed in claim 5 is characterized in that, described mixing device is the thread mixing Presoaker.
7. described specific equipment as claimed in claim 5, it is characterized in that, described screenings tripping device comprises screw squeezer, hydrolyzed solution surge tank, acid proof pump, valve and under meter, the liquid discharge port of screw squeezer is communicated with hydrolyzed solution surge tank opening for feed, hydrolyzed solution surge tank discharge port be connected by pipeline with the opening for feed of outlet pipe and mixing device respectively, be provided with acid proof pump, valve and under meter on this pipeline.
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| CN 201010598948 CN102021252B (en) | 2010-12-21 | 2010-12-21 | Method and device for continuously hydrolyzing corn bran |
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| CN102391065B (en) * | 2011-08-09 | 2014-02-05 | 山东省鲁洲食品集团有限公司 | Method for producing dihydric alcohol and low molecular polyalcohol by taking corn husk as raw material |
| CN104719627B (en) * | 2015-04-13 | 2018-01-19 | 山东省鲁洲食品集团有限公司 | It is a kind of can Direct-fed livestock and poultry corn steep liquor/dry powder processing method |
| CN107419035A (en) * | 2015-09-14 | 2017-12-01 | 山东富欣生物科技股份有限公司 | A kind of method that high-purity L arabinoses are prepared using maize peel as raw material continuously cooking |
| CN107447057B (en) * | 2016-05-31 | 2021-08-03 | 中国科学院大连化学物理研究所 | Biomass continuous hydrolysis and compression molding device |
| CN107447059A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院大连化学物理研究所 | A kind of biomass by hydrolyzation produces xylose mother liquid and residue compression forming integral method |
| CN109355443B (en) * | 2018-12-04 | 2020-07-17 | 浙江华康药业股份有限公司 | System and method for preparing xylose liquid by continuous hydrolysis of hemicellulose |
| CN114959263B (en) * | 2022-04-28 | 2023-02-07 | 北京科技大学 | Device and method for strengthening bioleaching by using acid to treat straws |
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