CN105132593A - Method for preparing crystalline fructose and crystal glucose from maize straw - Google Patents
Method for preparing crystalline fructose and crystal glucose from maize straw Download PDFInfo
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- CN105132593A CN105132593A CN201510596446.XA CN201510596446A CN105132593A CN 105132593 A CN105132593 A CN 105132593A CN 201510596446 A CN201510596446 A CN 201510596446A CN 105132593 A CN105132593 A CN 105132593A
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Abstract
The invention belongs to the technical field of crop treatment, and particularly relates to a method for preparing crystalline fructose and crystal glucose from maize straw. The method comprises the following steps: (1) pressing; (2) filtering; (3) clarificating and decolorizing; (4) concentrating; (5) chromatographing; (6) secondary concentrating; (7) crystallizing, separating and drying. According to the method, crystalline fructose and crystal glucose are prepared from fresh green maize straw, so that not only is the environmental problem caused by maize straw treatment solved to play the nutritional value of the maize straw to the utmost extent and obtain crystalline fructose and crystal glucose, but also the residue of the straw can serve as a feed to realize large-scale raising of cows, sheep and the like and generate a great economic benefit. Through cyclic utilization, the method can be widely applied to the fields of food, feeds and the like.
Description
Technical field
The invention belongs to the technical field of farm crop process, be specifically related to a kind of method utilizing maize straw to produce crystal diabetin and crystalline dextrose.
Background technology
Maize straw is the waste after corn maturation, then contains abundant nutritive ingredient in maize straw, and wherein containing total reducing sugar 12%, fructose accounts for 6%, and glucose sugar accounts for 6%; Simultaneously also containing a large amount of robust fibre, crude fat, crude protein and mineral substance etc.Process in the following ways under normal circumstances: (1) is as rubbish; (2) burn; (3) shatter.Carrying out processing as rubbish for mode (1) is waste to maize straw resource, cannot play it and be worth; Mode (2) is burned and is not only increased Carbon emission, causes environmental problem, and wastes resource; It is not obvious that mode (3) shatters treatment effect, because after pulverizing Exposure to Sunlight, stalk is stiff, is not suitable for sowing in its arable land, so can carry out burning disposal more again.Damage environment, utility value is very little.
Summary of the invention
The object of the invention is to cannot play the problem of its nutrition and economic worth for current maize straw processing mode and a kind of method utilizing maize straw to produce crystal diabetin and crystalline dextrose is provided, the method not only solves the environmental problem that maize straw process causes, and play its nutritive value to greatest extent, obtain crystal diabetin and crystalline dextrose, stalk slag can realize extensive raisings such as cattle and sheep as feed again simultaneously, produce great economic benefit, by recycle, the field such as food, feed can be widely used in.
Technical scheme of the present invention is: a kind of method utilizing maize straw to produce crystal diabetin and crystalline dextrose, comprises the following steps:
(1) squeeze: get fresh Green maize stalk and put into squeezing machine and carry out squeezing and obtain stalk Normal juice and stalk slag; Wherein first laterally squeezing, Green maize stalk enters squeezing machine with 7 ~ 12 °, more longitudinally squeezing, and Green maize stalk enters squeezing machine with 83 ~ 96 °;
(2) filter: step (1) gained stalk Normal juice is delivered to filter and filters, obtain pure straw juice and filter residue;
(3) clarify and decolorize: react 15 ~ 20 minutes add calcium hydroxide and volatile salt normal temperature in pure straw juice under; Then remove ammonia at being heated to 70 ~ 75 DEG C and add phosphoric acid and neutralize; Flocculation agent T is added at carrying out being heated to 100 ~ 105 DEG C again
1150, heavy sulphur oxygen and Poly Dimethyl Diallyl Ammonium Chloride, carry out decolouring also sedimentation and filtration isolate subsider juice; Wherein the weight part ratio of calcium hydroxide and volatile salt is 1.2 ~ 1.4:1; Flocculation agent T1150: heavy sulphur oxygen: Poly Dimethyl Diallyl Ammonium Chloride is 2:3:1.5 by weight;
(4) concentrated: step (3) gained subsider juice to be placed in quadruple effect falling-film evaporator and to carry out concentrating the heavy syrup obtaining 55 ~ 64%;
(5) chromatographic separation: the heavy syrup of step (4) gained is separated by chromatographic column, obtains fructose syrups and dextrose syrup respectively;
(6) secondary concentration: respectively the fructose syrups of step (5) gained and dextrose syrup are placed in five effect falling-film evaporators and concentrate, obtains concentration respectively and is the concentrated fructose syrups of 90 ~ 93% and concentrated dextrose syrup;
(7) crystallization, separation and drying: respectively fructose syrups is concentrated to step (6) gained and carry out crystallization with concentrated dextrose syrup, be separated and drying, obtain crystal diabetin and crystalline dextrose respectively; Wherein the crystallization condition of concentrated fructose syrups is: crystallization time 20 ~ 28 hours, and pH value is 3.7 ~ 4.5, and Tc is 46 ~ 64 DEG C, and terminal temperature is 24 ~ 36 DEG C; The crystallization condition of concentrated dextrose syrup is: crystallization time 8 ~ 12 hours, pH value is 3.2 ~ 4.5, and Tc is 44 ~ 46 DEG C, and terminal temperature is 22 ~ 30 DEG C.
Described step (1) squeezing gained stalk slag is filtered gained filter residue with described step (2) carry out being mixed to get mixing slag, then by this mixing slag through compression moulding, make cubed feed.Cubed feed nutritive ingredient is worth high, and cattle and sheep have eaten and have been easy to digestion, and volume only has 1/20 of loose grass, is applicable to long-distance transport and stores.
Described step (1) squeezing gained stalk slag and described step (2) are filtered gained filter residue to be mixed to get and to mix slag, this mixing slag is placed in massfraction be 1.5% sodium hydroxide react 0.5 ~ 1.5 hour at 75 ~ 79 DEG C, then 170 ~ 175 DEG C are warming up to, vapour is carried out quick-fried 10 minutes under 1.3 ~ 1.8MPa, vapour quick-fried rear to mixing slag carry out centrifugal, by centrifugal rear gained solid phase through washing after carry out enzymolysis.Through the oxygenation pretreatment then quick-fried enzymolysis again of vapour, whole method total reducing sugar yield is made to improve 11 ~ 19%.
Described enzymolysis is specially: enzymolysis concentration of substrate is 24 ~ 29g/L, and enzyme dosage is cellulase 33IU/g dry, fiber
Disaccharidase 18IU/g dry; Temperature is 47 ~ 53 DEG C, and pH value is 4.7 ~ 5.1, is hydrolyzed 44 ~ 50 hours.
In described step (7) crystallization, separation and drying, gained crystal diabetin and crystalline dextrose water content are all less than 0.08%.
In described step (7) crystallization, separation and drying, the saturation ratio of crystallization is 1.5 ~ 1.7.
The feed rate of described step (5) chromatographic separation is 10 ~ 37mL/min, and washing fluid flow is 75 ~ 118mL/min; In flushing process, liquid phase flow rate is 3.2 ~ 4.7mL/min, and fluid flow rate control is at 2.7 ~ 3.5mL/min; Separation temperature is 67 ~ 74 DEG C.
Beneficial effect of the present invention is: the method utilizing maize straw to produce crystal diabetin and crystalline dextrose of the present invention, adopts Physical in conjunction with biochemical process, makes corn stover be biological nutrient sugar and vegetable solid feed.The method gained crystal diabetin and crystalline dextrose purity is adopted to reach 99.6 ~ 99.8%; Crystallization yield reaches 78 ~ 85%; Percent of decolourization reaches 93 ~ 95.2%, occurs without color reversion phenomenon.
The economic benefit brought is specially: suppose that 0.07 hectare corn can produce 600 kilograms of corns, maize straw 4000 kilograms, and contain total reducing sugar 12% by stalk, wherein fructose accounts for 6%, and glucose accounts for 6% calculating, then can produce 200 kilograms, fructose, glucose 200 kilograms.By crystal diabetin market price 1.3 ~ 1.4 ten thousand yuan per ton, 2600 yuan can be taken in; Crystalline dextrose market price about 5,000, can take in 1000 yuan, adds up to every mu of maize straw output value 3600 yuan.Maize straw slag after extraction about 2000 kilograms, can make ox, sheep animal feed.For sheep, every sheep can with feed every day 1.5 kilograms, available 1300 days, deliver calculating in 300 days for sale by every sheep, 0.07 hectare maize straw can support 4 sheep, every only 40 kilograms, 4 take in 4800 yuan only, on corn basis, 600 kilograms, every mu of ground, increase by 8400 yuan of incomes again can to peasant.
In sum, the described method utilizing maize straw to produce crystal diabetin and crystalline dextrose not only solves the environmental problem that maize straw process causes, improve the ecological environment, and play to greatest extent its nutritive value and, and produce economic benefit, make increasing peasant income, pass through recycle, improve added value, can food, feed etc. be widely used in.
Embodiment
Below by embodiment, the present invention will be described in detail.
Embodiment 1
Utilize maize straw to produce a method for crystal diabetin and crystalline dextrose, comprise the following steps:
(1) squeeze: get fresh Green maize stalk and put into squeezing machine and carry out squeezing and obtain stalk Normal juice and stalk slag; Wherein first laterally squeezing, Green maize stalk enters squeezing machine with 7 ~ 12 °, more longitudinally squeezing, and Green maize stalk enters squeezing machine with 83 ~ 96 °;
(2) filter: step (1) gained stalk Normal juice is delivered to filter and filters, obtain pure straw juice and filter residue;
(3) clarify and decolorize: react 15 ~ 20 minutes add calcium hydroxide and volatile salt normal temperature in pure straw juice under; Then remove ammonia at being heated to 70 ~ 75 DEG C and add phosphoric acid and neutralize; Flocculation agent T is added at carrying out being heated to 100 ~ 105 DEG C again
1150, heavy sulphur oxygen and Poly Dimethyl Diallyl Ammonium Chloride, carry out decolouring also sedimentation and filtration isolate subsider juice; Wherein the weight part ratio of calcium hydroxide and volatile salt is 1.2 ~ 1.4:1; Flocculation agent T1150: heavy sulphur oxygen: Poly Dimethyl Diallyl Ammonium Chloride is 2:3:1.5 by weight;
(4) concentrated: step (3) gained subsider juice to be placed in quadruple effect falling-film evaporator and to carry out concentrating the concentrated sugar obtaining 55 ~ 64%
Slurry;
(5) chromatographic separation: the heavy syrup of step (4) gained is separated by chromatographic column, obtains fructose syrups and dextrose syrup respectively; Wherein feed rate is 10 ~ 37mL/min, and washing fluid flow is 75 ~ 118mL/min; In flushing process, liquid phase flow rate is 3.2 ~ 4.7mL/min, and fluid flow rate control is at 2.7 ~ 3.5mL/min; Separation temperature is 67 ~ 74 DEG C;
(6) secondary concentration: respectively the fructose syrups of step (5) gained and dextrose syrup are placed in five effect falling-film evaporators and concentrate, obtains concentration respectively and is the concentrated fructose syrups of 90 ~ 93% and concentrated dextrose syrup;
(7) crystallization, separation and drying: respectively to step (6) gained concentrate fructose syrups and concentrated dextrose syrup carry out crystallization,
Be separated and drying, obtain crystal diabetin and crystalline dextrose respectively; Wherein the crystallization condition of concentrated fructose syrups is: crystallization time
20 ~ 28 hours, pH value was 3.7 ~ 4.5, and Tc is 46 ~ 64 DEG C, and terminal temperature is 24 ~ 36 DEG C; Concentrated glucose
The crystallization condition of syrup is: crystallization time 8 ~ 12 hours, and pH value is 3.2 ~ 4.5, and Tc is 44 ~ 46 DEG C, terminal
Temperature is 22 ~ 30 DEG C, and the saturation ratio of crystallization is 1.5 ~ 1.7.Wherein gained crystal diabetin and crystalline dextrose water content are all less than 0.08%.
Described step (1) squeezing gained stalk slag is filtered gained filter residue with described step (2) carry out being mixed to get mixing slag, then by this mixing slag through compression moulding, make cubed feed.Cubed feed nutritive ingredient is worth high, and cattle and sheep have eaten and have been easy to digestion, and volume only has 1/20 of loose grass, is applicable to long-distance transport and stores.
Embodiment 2
Utilize maize straw to produce a method for crystal diabetin and crystalline dextrose, comprise the following steps:
(1) squeeze: get fresh Green maize stalk and put into squeezing machine and carry out squeezing and obtain stalk Normal juice and stalk slag; Wherein first laterally squeezing, Green maize stalk enters squeezing machine with 7 ~ 12 °, more longitudinally squeezing, and Green maize stalk enters squeezing machine with 83 ~ 96 °;
(2) filter: step (1) gained stalk Normal juice is delivered to filter and filters, obtain pure straw juice and filter residue;
(3) clarify and decolorize: react 15 ~ 20 minutes add calcium hydroxide and volatile salt normal temperature in pure straw juice under; Then add
Heat neutralizes to removing ammonia and add phosphoric acid at 70 ~ 75 DEG C; Flocculation agent is added at carrying out being heated to 100 ~ 105 DEG C again
T
1150, heavy sulphur oxygen and Poly Dimethyl Diallyl Ammonium Chloride, carry out decolouring also sedimentation and filtration isolate subsider juice; Wherein hydroxide
The weight part ratio of calcium and volatile salt is 1.2 ~ 1.4:1; Flocculation agent T1150: heavy sulphur oxygen: Poly Dimethyl Diallyl Ammonium Chloride
Be 2:3:1.5 by weight;
(4) concentrated: step (3) gained subsider juice to be placed in quadruple effect falling-film evaporator and to carry out concentrating the concentrated sugar obtaining 55 ~ 64%
Slurry;
(5) chromatographic separation: the heavy syrup of step (4) gained is separated by chromatographic column, obtains fructose syrups and dextrose syrup respectively; Wherein feed rate is 10 ~ 37mL/min, and washing fluid flow is 75 ~ 118mL/min; In flushing process, liquid phase flow rate is 3.2 ~ 4.7mL/min, and fluid flow rate control is at 2.7 ~ 3.5mL/min; Separation temperature is 67 ~ 74 DEG C;
(6) secondary concentration: respectively the fructose syrups of step (5) gained and dextrose syrup are placed in five effect falling-film evaporators and concentrate, obtains concentration respectively and is the concentrated fructose syrups of 90 ~ 93% and concentrated dextrose syrup;
(7) crystallization, separation and drying: respectively to step (6) gained concentrate fructose syrups and concentrated dextrose syrup carry out crystallization,
Be separated and drying, obtain crystal diabetin and crystalline dextrose respectively; Wherein the crystallization condition of concentrated fructose syrups is: crystallization time
20 ~ 28 hours, pH value was 3.7 ~ 4.5, and Tc is 46 ~ 64 DEG C, and terminal temperature is 24 ~ 36 DEG C; Concentrated glucose
The crystallization condition of syrup is: crystallization time 8 ~ 12 hours, and pH value is 3.2 ~ 4.5, and Tc is 44 ~ 46 DEG C, terminal
Temperature is 22 ~ 30 DEG C, and the saturation ratio of crystallization is 1.5 ~ 1.7.Wherein gained crystal diabetin and crystalline dextrose water content all little
In 0.08%.
Described step (1) squeezing gained stalk slag and described step (2) are filtered gained filter residue to be mixed to get and to mix slag, this mixing slag is placed in massfraction be 1.5% sodium hydroxide react 0.5 ~ 1.5 hour at 75 ~ 79 DEG C, then 170 ~ 175 DEG C are warming up to, vapour is carried out quick-fried 10 minutes under 1.3 ~ 1.8MPa, vapour quick-fried rear to mixing slag carry out centrifugal, centrifugal rear gained solid phase is carried out enzymolysis after washing, enzymolysis concentration of substrate is 24 ~ 29g/L, enzyme dosage is cellulase 33IU/g dry, cellobiase 18IU/g dry; Temperature is 47 ~ 53 DEG C, and pH value is 4.7 ~ 5.1, is hydrolyzed 44 ~ 50 hours.。Through the oxygenation pretreatment then quick-fried enzymolysis again of vapour, whole method total reducing sugar yield is made to improve 11 ~ 19%.
Claims (7)
1. utilize maize straw to produce a method for crystal diabetin and crystalline dextrose, comprise the following steps:
(1) squeeze: get fresh Green maize stalk and put into squeezing machine and carry out squeezing and obtain stalk Normal juice and stalk slag; Wherein first laterally squeezing, Green maize stalk enters squeezing machine with 7 ~ 12 °, more longitudinally squeezing, and Green maize stalk enters squeezing machine with 83 ~ 96 °;
(2) filter: step (1) gained stalk Normal juice is delivered to filter and filters, obtain pure straw juice and filter residue;
(3) clarify and decolorize: react 15 ~ 20 minutes add calcium hydroxide and volatile salt normal temperature in pure straw juice under; Then remove ammonia at being heated to 70 ~ 75 DEG C and add phosphoric acid and neutralize; Flocculation agent T is added at carrying out being heated to 100 ~ 105 DEG C again
1150, heavy sulphur oxygen and Poly Dimethyl Diallyl Ammonium Chloride, carry out decolouring also sedimentation and filtration isolate subsider juice; Wherein the weight part ratio of calcium hydroxide and volatile salt is 1.2 ~ 1.4:1; Flocculation agent T1150: heavy sulphur oxygen: Poly Dimethyl Diallyl Ammonium Chloride is 2:3:1.5 by weight;
(4) concentrated: step (3) gained subsider juice to be placed in quadruple effect falling-film evaporator and to carry out concentrating the heavy syrup obtaining 55 ~ 64%;
(5) chromatographic separation: the heavy syrup of step (4) gained is separated by chromatographic column, obtains fructose syrups and dextrose syrup respectively;
(6) secondary concentration: respectively the fructose syrups of step (5) gained and dextrose syrup are placed in five effect falling-film evaporators and concentrate, obtains concentration respectively and is the concentrated fructose syrups of 90 ~ 93% and concentrated dextrose syrup;
(7) crystallization, separation and drying: respectively fructose syrups is concentrated to step (6) gained and carry out crystallization with concentrated dextrose syrup, be separated and drying, obtain crystal diabetin and crystalline dextrose respectively; Wherein the crystallization condition of concentrated fructose syrups is: crystallization time 20 ~ 28 hours, and pH value is 3.7 ~ 4.5, and Tc is 46 ~ 64 DEG C, and terminal temperature is 24 ~ 36 DEG C; The crystallization condition of concentrated dextrose syrup is: crystallization time 8 ~ 12 hours, pH value is 3.2 ~ 4.5, and Tc is 44 ~ 46 DEG C, and terminal temperature is 22 ~ 30 DEG C.
2. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 1, it is characterized in that, described step (1) squeezing gained stalk slag is filtered gained filter residue with described step (2) carry out being mixed to get mixing slag, then by this mixing slag through compression moulding, make cubed feed.
3. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 1, it is characterized in that, described step (1) squeezing gained stalk slag and described step (2) are filtered gained filter residue to be mixed to get and to mix slag, this mixing slag is placed in massfraction be 1.5% sodium hydroxide react 0.5 ~ 1.5 hour at 75 ~ 79 DEG C, then 170 ~ 175 DEG C are warming up to, vapour is carried out quick-fried 10 minutes under 1.3 ~ 1.8MPa, vapour quick-fried rear to mixing slag carry out centrifugal, by centrifugal rear gained solid phase through washing after carry out enzymolysis.
4. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 3, it is characterized in that, described enzymolysis is specially: enzymolysis concentration of substrate is 24 ~ 29g/L, and enzyme dosage is cellulase 33IU/g dry, cellobiase 18IU/g dry; Temperature is 47 ~ 53 DEG C, and pH value is 4.7 ~ 5.1, is hydrolyzed 44 ~ 50 hours.
5. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 1, it is characterized in that, in described step (7) crystallization, separation and drying, gained crystal diabetin and crystalline dextrose water content are all less than 0.08%.
6. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 1, it is characterized in that, in described step (7) crystallization, separation and drying, the saturation ratio of crystallization is 1.5 ~ 1.7.
7. utilize maize straw to produce the method for crystal diabetin and crystalline dextrose according to claim 1, it is characterized in that, the feed rate of described step (5) chromatographic separation is 10 ~ 37mL/min, and washing fluid flow is 75 ~ 118mL/min; In flushing process, liquid phase flow rate is 3.2 ~ 4.7mL/min, and fluid flow rate control is at 2.7 ~ 3.5mL/min; Separation temperature is 67 ~ 74 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106282422A (en) * | 2016-08-31 | 2017-01-04 | 呼伦贝尔东北阜丰生物科技有限公司 | A kind of method of separation and Extraction glucose from starch saccharificating liquid |
| CN110303024A (en) * | 2018-03-20 | 2019-10-08 | 郑庆义 | A kind of straw method of comprehensive utilization |
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| CN104152589A (en) * | 2013-05-13 | 2014-11-19 | 广西工学院 | Ammonium carbonate salt-based cane sugar juice clarifying, decolouring and decontaminating method |
| CN104673942A (en) * | 2015-02-11 | 2015-06-03 | 广东永青生物科技有限公司 | Method for producing crystalline fructose from sucrose |
| CN104837376A (en) * | 2012-08-20 | 2015-08-12 | 天然成分有限责任公司 | Method of producing a sugar product from fruit |
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2015
- 2015-09-18 CN CN201510596446.XA patent/CN105132593A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| CN1218838A (en) * | 1997-12-03 | 1999-06-09 | 钱永淋 | Natural fructose and natural glucose and their preparing method |
| CN101548023A (en) * | 2006-11-08 | 2009-09-30 | 通加特休利特有限公司 | Treatment of sugar juice |
| CN101638695A (en) * | 2009-08-24 | 2010-02-03 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of crystalline fructose |
| CN104837376A (en) * | 2012-08-20 | 2015-08-12 | 天然成分有限责任公司 | Method of producing a sugar product from fruit |
| CN104152589A (en) * | 2013-05-13 | 2014-11-19 | 广西工学院 | Ammonium carbonate salt-based cane sugar juice clarifying, decolouring and decontaminating method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106282422A (en) * | 2016-08-31 | 2017-01-04 | 呼伦贝尔东北阜丰生物科技有限公司 | A kind of method of separation and Extraction glucose from starch saccharificating liquid |
| CN110303024A (en) * | 2018-03-20 | 2019-10-08 | 郑庆义 | A kind of straw method of comprehensive utilization |
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