CN109402195B - A kind of method of continuous liquefaction high concentration starch - Google Patents
A kind of method of continuous liquefaction high concentration starch Download PDFInfo
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- CN109402195B CN109402195B CN201711063588.5A CN201711063588A CN109402195B CN 109402195 B CN109402195 B CN 109402195B CN 201711063588 A CN201711063588 A CN 201711063588A CN 109402195 B CN109402195 B CN 109402195B
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- starch
- amylase
- lipase
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- diastase
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
Abstract
The present invention provides a kind of methods for carrying out continuous liquefaction processing to high concentration cornstarch using injection liquefaction technology, by the way that medium temperature amylase, alpha-amylase, lipase and protease is applied in combination, and two-step method is preferably implemented and is continuously liquefied, the viscosity of starch during Heat Gelatinization is effectively reduced, so as to handle under lower steam jeting pressure the starch milk of high concentration.According to the method for the present invention, liquefier dry matter content is up to 40-70wt%, and protein flocculation phenomenon is obvious after liquefaction, and the saccharified liquid rate of filtration obtained after liquefaction is fast, and saccharified liquid is limpid.
Description
Technical field
The invention belongs to starch sugaring processing technique fields, and in particular to a kind of continuously to be sprayed using steam direct heating
The method of liquefaction high concentration starch.
Background technique
Starch sugar is the important source material of China's food industry, is the useful supplement of people's current consumption sugar, therefore is improved
The quality of starchy carbohydrate product, reducing production cost is particularly important.In recent years, enzymatic hydrolysis sugar refining technology gradually replaces
Acid system sugar refining technology.However, the increase of viscosity is so that liquefaction control becomes when starch milk initial concentration increases
Difficulty, thus it is industrial at present usually by the control of starch milk initial concentration in 25%-30%.However, subsequent saccharifying needs
Saccharified liquid is concentrated using evaporation, therefore lower starch milk initial concentration makes saccharifying huge energy consumption.
Enzymatic hydrolysis sugaring is generally divided into two steps, first using the strong amylase of specificity by starch liquefacation, followed by
Dextrin or the further hydrolysis of oligosaccharide are glucose by carbohydrase.Enzyme process reaction condition is mild, and side reaction is few, conversion effect
Rate is high.However the enzyme digestion reaction time is longer, and since enzyme is protein, easily causes filtration difficulty.
Commonly used starch liquefying process is injection liquefaction technology at present.Injection liquefaction technology generally comprises pre liquefied
Processing stage and liquefaction processing stage.Starch is generally added water to size mixing into starch milk by pretreatment stage, and starch is added after adjusting pH
The protective agent and activator of enzyme are eventually adding high temperature resistant α-amylase.In liquefaction processing stage, the starch milk that will be stirred evenly
Jet liquefier is squeezed into, so that the starch milk ejected is directly contacted with high-temperature steam.For the work for meeting Thermostable α-Amylase
Property and injection liquefaction duty requirements, usually the temperature of steam is controlled between 90-120 DEG C, and its pressure is controlled in 0.9-
Between 1.2MPa.Injection liquefaction technology heats rapidly starch milk using high-temperature steam, and it is viscous can to limit starch in a short time
Degree increases.However, at the temperature disclosed above, starch gelatinization phenomenon is still extremely serious, viscosity is clearly demarcated to the limitation still ten of technique
It is aobvious, therefore be generally also difficult to the initial concentration of starch milk being increased to 35% or more.On the other hand, when using indirect heating,
Starch heated time is too long, causes liquefaction fluid viscosity excessively high, so that pumping and processing later are sufficiently complex.
A kind of method of continuous liquefaction high concentration starch is disclosed in CN104520333A.In the pre liquefied stage, in 25-
The enzyme that one or more degradable starch are added in the first starch milk of 45wt%, obtains pre liquefied product；In liquefaction stage,
Starch is added in first starch milk, dry matter content is obtained in the second starch milk of 30-80wt%, is then moved from reactor
Except a part of the second starch milk, it is sent to liquefaction step, and by continuing to add starch, maintains the dry of the second starch milk
Content of material.Since there are degradable starch, compared with traditional technology, the dry matter content of the second starch milk is higher, without
It leads to the problem of and is gelatinized and viscosity increases.In addition, by way of using indirect heating (welded plate type heat exchanger) to starch milk
It liquefies, the moisture for avoiding high-temperature steam from bringing into.However, this method can not make the uniform disperse system of Starch formation, obtain
The equal existing defects of the sugared rate of the liquefier filterability and starch that arrive.
As it can be seen that the increase of viscosity directly limits contents on dry basis after starch milk initial concentration and liquefaction after starch gelatinization, because
This increases industrial energy consumption.To solve above-mentioned viscosity problem, a kind of promotion high concentration starch fluid is disclosed in CN104293863A
The preprocess method of change.This method adds the mesophilicα-diastase of 0.075-1U/g starch in the starch of 35-60wt%,
5-30min is pre-processed at 55-60 DEG C；In liquefaction stage, remaining mesophilicα-diastase cooperates with Thermostable α-Amylase liquefaction portion
Divide starch, further decreases liquefaction process viscosity.The above method makes high concentration by reduction gelatinization and the viscosity of liquefaction process
Starch High-temperature Liquefaction is gone on smoothly.
For the whole embodiments of the above method, embodiment 1-3 is that deionized water dilution is added in pretreatment fluid
(that is, water of 4 times of addition) row measurement again after to 20%, only embodiment 4 is directly to be measured to pretreatment fluid.Due to starch
There is no stringent proportional relation, excess dilution not only directly contributes the quality of starch in starch milk for newborn viscosity and dilution ratio
Score reduces, the confidence level decline for the viscosity data that also it can be made to measure.It is compared with the control group, pre- to locate according to embodiment 1-3
The liquefier peak viscosity of reason group has dropped 25-33%, and in embodiment 4, compared with the control group, the liquefier of pretreated group
Peak viscosity only has dropped about 7%.As it can be seen that this method in fact and solution high-concentration starch milk not yet in effect gelatinization, liquefaction process
The problem of middle excessive concentration.
CN104911234A provides the method for similar substep liquefaction high concentration cornstarch.This method is with 40%-
65% high concentration corn starch milk is reaction substrate, and the medium temperature α-of 6-28U/g starch is added into uniform starch milk of sizing mixing
Amylase carries out the liquefaction of first time medium temperature amylase；And it is added into the liquefier after first mesophilicα-diastase liquefaction
High temperature resistant α-amylase of 8-30U/g starch, to obtain the liquefier for being suitble to saccharification.As can be seen that the medium temperature α-of this method
Amylase is 6-370 times of CN104293863A method, the liquefier that just can be properly saccharified.
Therefore, there are still the demands to starch liquefacation technological improvement for this field.
Summary of the invention
In a first aspect, the present invention provides it is a kind of promote high concentration starch liquefacation preprocess method, the method packet
Containing following steps: using the starch milk of 38-55wt% as substrate, medium temperature α-amylase, Thermostable α-Amylase, fat is added
Enzyme and neutral proteinase are kept the temperature after mixing at 45-60 DEG C.
In second aspect, the present invention provides a kind of methods using steam direct heating liquefaction high concentration starch, wherein
It the described method comprises the following steps:
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0,
Mesophilicα-diastase, Thermostable α-Amylase, lipase and neutral proteinase is added, keeps the temperature, obtains at 45-60 DEG C after mixing
Brix value is the first starch milk of 9-18%；
(2) first starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is dodged
It steams, cools the temperature to 97-99 DEG C, then keep the temperature 0.5h-3h at 95-97 DEG C, obtain liquefier；Wherein, the injection liquefaction
In, the temperature of jet port is 100-110 DEG C, steam pressure 0.5-0.7MPa.
In the third aspect, continuously liquefied using injection liquefaction technology to high concentration starch the present invention provides a kind of
The method of processing, the method comprises the following steps:
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0,
Mesophilicα-diastase, Thermostable α-Amylase, lipase and neutral proteinase is added, keeps the temperature, obtains at 45-60 DEG C after mixing
Brix value is the first starch milk of 9-18%；
(2) starch that butt quality score > 70% is added is stirred in the first starch milk of Xiang Suoshu, obtains butt quality point
Number is the second starch milks of 50-70wt%, be added in the second starch milk of Xiang Suoshu mesophilicα-diastase, Thermostable α-Amylase,
Lipase and neutral proteinase obtain the third that brix value is 10%-24% and form sediment in 50-60 DEG C of heat preservation 0.5h or more after mixing
Powder cream；And
(3) the third starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is dodged
It steams, cools the temperature to 97-99 DEG C, then keep the temperature 0.5h-3h at 95-97 DEG C, obtain liquefier；It is liquefied in the injection
Meanwhile Xiang Suoshu sizes mixing and supplements starch, water and mesophilicα-diastase, the high temperature resistant α-shallow lake of butt quality score > 70% in tank
Powder enzyme, lipase and neutral proteinase；Wherein, in the injection liquefaction, the temperature of jet port is 100-110 DEG C, steam pressure
For 0.5-0.7MPa；Wherein, the starch and water supplemented makes the butt quality score of material in the tank of sizing mixing to be
50wt%-70wt%.
Beneficial effect
The present invention effectively reduces heating paste by alpha-amylase, lipase and protease mild in being applied in combination
The viscosity of starch during change.In turn, in a preferred embodiment, by implementing two-step method and continuous liquefaction, more
Significantly reduce the viscosity of starch during Heat Gelatinization, so as under lower steam jeting pressure to high concentration
Starch milk handled.According to the method for the present invention, liquefier dry matter content is up to 40-70wt%；DE value is in 22-28.
In turn, in continuous liquefied embodiment, liquefier dry matter content is up to 50-70wt%.Protein flocculation is existing after liquefaction
As obvious, albumen precipitation floats on saccharified liquid surface, therefore the saccharified liquid rate of filtration obtained after liquefying is fast, and saccharified liquid is limpid,
Impurity is less, conducive to the progress of later period separation process.The present invention uses the injection liquefaction technology of steam direct heating, and realizes
The continuous liquefaction of high concentration starch.
Detailed description of the invention
Fig. 1 shows the result being measured to the viscosity of the first starch milk of embodiment 1 and comparative example 1,2,3.
Specific embodiment
It hereafter will be apparent from the present invention.
Processing cornstarch is carried out using method of the invention, is particularly grain in storage for years corn.With grain in storage for years corn
As in the embodiment of raw material, preferably in step (1), the starch milk that butt quality score is 38-55wt% is prepared.
In a first aspect, the present invention provides it is a kind of promote high concentration starch liquefacation preprocess method, the method packet
Containing following steps: using the starch milk of 38-55wt% as substrate, medium temperature α-amylase, Thermostable α-Amylase, fat is added
Enzyme and neutral proteinase are kept the temperature after mixing at 45-60 DEG C.
Preferably, the mesophilicα-diastase, the Thermostable α-Amylase, the lipase and the neutral protein
Enzyme is added by following ratio: in terms of starch on dry basis, 0.1 ‰ -0.4 ‰ medium temperature α-amylase, 0.2 ‰ -0.3 ‰ resistance to height
The neutral proteinase of warm alpha-amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰.
In second aspect, the present invention provides a kind of methods using steam direct heating liquefaction high concentration starch, wherein
It the described method comprises the following steps:
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0,
Mesophilicα-diastase, Thermostable α-Amylase, lipase and neutral proteinase is added, keeps the temperature, obtains at 45-60 DEG C after mixing
Brix value is the first starch milk of 9-18%；
(2) first starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is dodged
It steams, cools the temperature to 97-99 DEG C, then keep the temperature 0.5h-3h at 95-97 DEG C, obtain liquefier；Wherein, the injection liquefaction
In, the temperature of jet port is 100-110 DEG C, steam pressure 0.5-0.7MPa.
For step (1), it is preferable that the preparation of starch milk 45-60 DEG C at a temperature of carry out.Preferably, in described
Warm alpha-amylase, the Thermostable α-Amylase, the lipase and the neutral proteinase are added with following ratio: with
Starch on dry basis meter, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase, 0.04-0.08 ‰
Lipase and 0.07-0.12 ‰ neutral proteinase.
For step (2), it is preferable that with 0.1-0.2m3The speed of/h pumps the first starch milk.
In the third aspect, the present invention provides a kind of continuously to be liquefied the method for high concentration starch using steam direct heating,
The method comprises the following steps:
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0,
Mesophilicα-diastase, Thermostable α-Amylase, lipase and neutral proteinase is added, keeps the temperature, obtains at 45-60 DEG C after mixing
Brix value is the first starch milk of 9-18%；
(2) starch that butt quality score > 70% is added is stirred in the first starch milk of Xiang Suoshu, obtains butt quality point
Number is the second starch milks of 50-70wt%, be added in the second starch milk of Xiang Suoshu mesophilicα-diastase, Thermostable α-Amylase,
Lipase and neutral proteinase obtain the third that brix value is 10%-24% and form sediment in 50-60 DEG C of heat preservation 0.5h or more after mixing
Powder cream；And
(3) the third starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is dodged
It steams, cools the temperature to 97-99 DEG C, then keep the temperature 0.5h-3h at 95-97 DEG C, obtain liquefier；It is liquefied in the injection
Meanwhile Xiang Suoshu sizes mixing and supplements starch, water and mesophilicα-diastase, the high temperature resistant α-shallow lake of butt quality score > 70% in tank
Powder enzyme, lipase and neutral proteinase；Wherein, in the injection liquefaction, the temperature of jet port is 100-110 DEG C, steam pressure
For 0.5-0.7MPa；Wherein, the starch and water supplemented makes the butt quality score of material in the tank of sizing mixing to be
50wt%-70wt%.
In step (1), by the first pretreatment, first is carried out to the starch milk that butt quality score is 38-55wt%
Pre liquefied obtains the first pre liquefied product (that is, first starch milk), which has the brix of 9%-18%
Value.Brix value has meaning well known in the art.Brix value has reacted the concentration of lipid soluble solid content.Preferably, starch
Cream preparation 45-60 DEG C at a temperature of carry out.In a preferred embodiment, mesophilicα-diastase when the first pre liquefied, resistance to
High-temperatureα-amylase, lipase and neutral proteinase are added by following ratio: in terms of starch on dry basis, 0.1 ‰ -0.4 ‰
Mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰
Neutral proteinase.By using enzymatic mixture, while pre liquefied starch milk, moreover it is possible to the viscosity of starch milk be effectively reduced.It can
Mesophilicα-diastase 480-B can be believed for Novi for mesophilicα-diastase of the invention, Thermostable α-Amylase can be Jie Neng section
High temperature resistant α-amylase POWERLIQ, lipase can be Shandong Longke Enzyme Co., Ltd.'s lipase, neutral proteinase
PWN10160 medium temperature protease can be believed for Novi.In order to balance the optimum activity condition of each enzyme, which exists
PH, 45-60 DEG C of progress of 5.0-6.0.Preferably, the first pre liquefied step carries out 0.5-3h.
In step (2), by the way that starch is added into the first pre liquefied product and carries out the second pre liquefied.Preferably, exist
Mesophilicα-diastase, Thermostable α-Amylase, lipase and the neutral proteinase being added in second pre liquefied are as follows: form sediment with second
The starch on dry basis meter of powder cream, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase, 0.04-
0.08 ‰ lipase and the neutral proteinase of 0.07-0.12 ‰.The third starch milk that second pre liquefied obtains has 10%-
24% brix value.
In step (3), starch and water are continuously supplemented into tank of sizing mixing while spraying liquefaction, realizes starch milk
Continuous liquefaction.Although feed liquid in tank of sizing mixing has the contents on dry basis of 50wt%-70wt%, due to two step pre liquefied, the
The viscosity of three starch milks is not too high, and pressure needed for injection liquefaction is only 0.5-0.7MPa.Preferably, the medium temperature supplemented
Alpha-amylase, high temperature resistant α-amylase, lipase and neutral proteinase are as follows: in terms of the starch on dry basis supplemented, 0.1 ‰-
0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase, 0.04-0.08 ‰ lipase and 0.07-
0.12 ‰ neutral proteinase.Preferably, in injection liquefaction, with 0.1-0.2m3The speed of/h pumps third starch
Cream.Preferably, starch is supplemented into tank of sizing mixing with the speed of 110-120kg/h.Preferably, with the speed of 80-90kg/h to tune
Water is supplemented in slurry tank.Steam is spurted into starch milk film using injector, can quickly be risen by injector in a short time
Temperature and complete gelatinization, liquefaction, disperse insoluble starch particle at high temperature, quantity is also greatly reduced, to make resulting
Liquefier is not only transparent but also is easy to filter, and the sugared rate of starch is also high.In addition, liquefier can be carried out into one by using flash distillation
Step concentration.
In highly preferred embodiment, the continuous liquifying method of starch of the invention is comprised the following steps:
(1) starch milk that butt quality score is 38wt%-55wt% is prepared in 50 DEG C of tank of sizing mixing, and pH is adjusted
To 6.0, in terms of starch on dry basis, Xiang Suoshu sizes mixing the resistance to height of mesophilicα-diastase, 0.2-0.3 ‰ that 0.1-0.4 ‰ is added in tank
The neutral proteinase of warm alpha-amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰, in 55 DEG C of heat preservation 0.5- after mixing
1h obtains the first starch milk that brix value is 9%-18%；
(2) starch that butt quality score > 80% is added is stirred in the first starch milk of Xiang Suoshu, obtains butt quality point
Number is the second starch milks of 50-70wt%, and Xiang Suoshu sizes mixing, and mesophilicα-diastase, the 0.2- of 0.1-0.4 ‰ are added in tank
The neutral proteinase of 0.3 ‰ Thermostable α-Amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰, after mixing
55 DEG C of heat preservation 0.5h or more obtain the third starch milk that brix value is 10%-24%；And
(3) with 0.1-0.2m3The third starch milk is carried out injection liquefaction through pipeline discharge by/h, to the injection liquid
Change product to be flashed, cools the temperature to 97-99 DEG C, then keep the temperature 1h-3h at 95-97 DEG C, obtain liquefier；Described
While injection liquefaction, Xiang Suoshu size mixing supplement in tank butt quality score > 70% starch, water and mesophilicα-diastase,
Thermostable α-Amylase, lipase and neutral proteinase；Wherein, in the injection liquefaction, the temperature of jet port is 100-110
DEG C, steam pressure 0.5-0.7MPa；Wherein, starch is supplemented into tank of sizing mixing with the speed of 110-120kg/h, and with 80-
The speed of 90kg/h supplements water into tank of sizing mixing, so that the starch and water that are supplemented make the butt of material in the tank of sizing mixing
Mass fraction is 50wt%-70wt%；Wherein, the mesophilicα-diastase that is supplemented, Thermostable α-Amylase, lipase and in
Property protease are as follows: in terms of the starch on dry basis supplemented, the high temperature resistant α-of the mesophilicα-diastase of 0.1-0.4 ‰, 0.2-0.3 ‰
The neutral proteinase of amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰.
Preferably, liquefier obtained has the dry matter content of the DE value of 22-28,50wt%-70wt%.DE value
It is glucose equivalent with meaning well known in the art, expression is that reduced sugar (with glucose meter) accounts for the hundred of syrup dry matter
Divide ratio.
Embodiment
It is better understood the present invention by means of following embodiments, these embodiments are only used for illustrating the present invention, no
It should be interpreted limitation of the present invention.
The steam injection equipment that embodiment uses is purchased from Shanghai Xiao Ledong tide biotechnology development corporation, Ltd., model
ESCS-M104.High-grade maize starch used in embodiment is purchased from China Oil and Food Import and Export Corporation's biochemistry energy (Gongzhuling) Co., Ltd, and butt contains
Amount is 87%.Mesophilicα-diastase believes (China) Bioisystech Co., Ltd, article No. 480-B purchased from Novi；High temperature resistant α-shallow lake
Powder enzyme is purchased from Jie Neng section (China) bioengineering Co., Ltd (article No. POWERLIQ)；Lipase is purchased from Shandong Long Kete enzyme system
Agent Co., Ltd lipase, neutral proteinase believe (China) Bioisystech Co., Ltd, article No. PWN10160 purchased from Novi.
In an embodiment of the present invention, the measuring method of sample liquid DE value is as follows:
1. solution is prepared
(a) methylene blue indicator solution (10g/L): weighing methylene blue 1.0g, is dissolved in water and is settled to 100mL.
(b) 100 ± 2 DEG C of benchmark DEXTROSE ANHYDROUSs that drying to constant weight glucose standards solution (2g/L): are weighed
0.5000g (claims standard to 0.0001g), is dissolved in water and is settled to 250mL.
(c) Fehling's solution is prepared
Fehling's solution I: copper sulphate (CuSO is weighed4·5H2O) 69.3g is dissolved in water and is settled to 1000mL, stores in palm fibre
In color bottle；
Fehling's solution II: sodium potassium tartrate tetrahydrate (KNaC is weighed4H4O6·4H2O) 346.0g and sodium hydroxide 100.0g, adds water
1000mL is dissolved and be settled to, is stored in rubber stopper vial.If having precipitating using preceding, supernatant use is drawn；
2. calibration: when pre- titration, successively drawing Fehling's solution II, each 5.0mL of Fehling's solution I in conical flask, add water
20mL is added bead 3, and glucose standards solution 24mL is added, shakes up solution in conical flask, and conical flask is heated, and controls
Solution processed boiling in 120 ± 15s, and keep slightly boiled, methylene blue indicator solution 2 is added and drips, continues with glucose standards solution
Titration, until it is its terminal that blue, which just disappears, entire titration operation should be completed in 3min.It is pre- to be added when formal titration
Glucose standards solution 1mL fewer than the glucose standards solution of above-mentioned titration consumption does parallel test, record consumption grape
The total volume of Standard for Sugars takes its arithmetic mean of instantaneous value.
The quality of consumption of glucose when 5mL each according to formula (1) calculating Fehling's solution II, I:
In formula:
The quality of consumption of glucose, g when each 5mL of RP: Fehling's solution II, I；
m1: weigh the amount of benchmark DEXTROSE ANHYDROUS, g；
V1: the total volume of consumption of glucose standard solution, mL.
3. measuring the DE value in sample liquid
(a) preparation of sample liquid
A certain amount of sample liquid is weighed, sampling amount contains reduction sugar amount to meet titration for condition in every 100mL sample liquid
125-200mg (claims standard to be advisable to 0.0001g), adds hot water dissolving, and be settled to 250mL with water.
(b) pre- titration
Fehling's solution II, each 5.0mL of Fehling's solution I are successively drawn in conical flask, adds water 20mL, bead 3 is added
Grain, it is pre- that part sample liquid is added, conical flask, the boiling in 120 ± 15s of control solution are heated, and keep slightly boiled, was dripped with every 2 seconds 1
Speed sample liquid is added dropwise, until when solution blue will disappear, methylene blue indicator solution 2 is added and drips, be further continued for that sample liquid is added dropwise until
It is its terminal, the total volume of record consumption sample liquid that blue, which just disappears,.
(c) formal titration
It is 1mL fewer than pre- titration sample liquid in being added in conical flask successively to draw Fehling's solution II, each 5.0mL of Fehling's solution I
Sample liquid heat conical flask, the boiling in 120 ± 15s of control solution in conical flask, and slight boiling condition is kept, with every 2 seconds 1
Sample liquid is added dropwise in the speed of drop, until methylene blue indicator solution 2 is added and drips when solution blue will disappear, it is straight to be further continued for dropwise addition sample liquid
Just disappearing to blue is its terminal, and entire titration operation must be completed in 3min, the total volume of record consumption sample liquid, according to
Formula (2) calculates the DE value in sample liquid:
In formula:
DE value: dextrose equivalent value in sample liquid, %；
The quality of consumption of glucose, g when each 5mL of RP: Fehling's solution II, I；
m2: sampling amount, g；
V2: the total volume of sample liquid, mL are consumed when titration；
DMC: the content of syrup dry matter (solid content), % in sample liquid.The DMC is also referred to as brix value in the art.
In an embodiment of the present invention, the measuring method of sample liquid DMC/brix value includes:
1. instrumental correction
At 20 DEG C, it is to steam the index of refraction of distilled water correction abbe's refractometer (precision is 0.0001 unit) again
1.3330, being equivalent to dry matter (solid content) soluble carbohydrate material content is zero, i.e., brix value is 0.
2. measuring DMC/brix value
(a) refractometer prism is opened, a small amount of sample liquid (1-2 drop) is added dropwise in prism facets center, rapid closing rib with glass bar
Mirror.Sample liquid is set uniformly to be covered with prism facets, bubble-free is simultaneously full of the visual field.
(b) constant temperature reads index of refraction (reading quasi- to 0.0001) and dry matter (solid) by eyepiece to 20.0 ± 0.1 DEG C
Soluble carbohydrate material percentage composition, i.e. sample liquid brix value.
Embodiment 1:
(1) using commercially available cornstarch as raw material, it is 45wt%'s that butt quality score is prepared in 50 DEG C of tank of sizing mixing
PH is adjusted to 6.0 with 8M hydrochloric acid by starch milk, in terms of starch on dry basis, Xiang Suoshu size mixing be added in tank 0.15 ‰ medium temperature α-shallow lake
Powder enzyme, 0.2 ‰ Thermostable α-Amylase, 0.04 ‰ lipase and 0.07 ‰ neutral proteinase, after mixing 55 DEG C protect
Warm 0.5h obtains the first starch milk that brix value is 15%；
(2) first starch milk is subjected to injection liquefaction through pipeline discharge, the temperature of jet port is 108 DEG C and maintains
3 minutes in pipe, steam pressure 0.6MPa.The injection liquefaction products are flashed, cool the temperature to 98 DEG C, then
2h is kept the temperature at 95 DEG C, obtains liquefier.
After measured, the liquefier DE value of acquisition is 25, and protein flocculates and swims on liquefier.With No. 101 150mm
The filtering of diameter filter paper, the rate of filtration are that every 4min filters out 75mL.
Embodiment 2:
(1) using commercially available cornstarch as raw material, it is 40wt%'s that butt quality score is prepared in 50 DEG C of tank of sizing mixing
PH is adjusted to 6.0 with 8M hydrochloric acid by starch milk, in terms of starch on dry basis, Xiang Suoshu size mixing be added in tank 0.25 ‰ medium temperature α-shallow lake
Powder enzyme, 0.2 ‰ Thermostable α-Amylase, 0.06 ‰ lipase and 0.1 ‰ neutral proteinase, after mixing 55 DEG C protect
Warm 1h obtains the first starch milk that brix value is 15%；
(2) cornstarch is added in stirring in the first starch milk of Xiang Suoshu, obtains second that butt quality score is 55wt%
Starch milk, Xiang Suoshu sizes mixing, and 0.25 ‰ mesophilicα-diastase, 0.2 ‰ Thermostable α-Amylase, 0.06 ‰ are added in tank
Lipase and 0.1 ‰ neutral proteinase obtain the third that brix value is 24% and form sediment in 55 DEG C of heat preservation 0.5h or more after mixing
Powder cream；
(3) with 0.18m3The third starch milk is carried out injection liquefaction through pipeline discharge by/h, and the temperature of jet port is
It 108 DEG C and maintains in pipe 3 minutes, steam pressure 0.6MPa.The injection liquefaction products are flashed, temperature is dropped
To 98 DEG C, 2h then is kept the temperature at 95 DEG C, obtains liquefier；While spraying liquefaction, with the speed of 85kg/h to the tune
Water is supplemented in slurry tank；Cornstarch is supplemented into the tank of sizing mixing with the speed of 114.8kg/h, while being supplemented in 0.25 ‰
Warm alpha-amylase, 0.2 ‰ Thermostable α-Amylase, 0.06 ‰ lipase and 0.1 ‰ neutral proteinase it is (dry with starch
Base meter), realize consecutive spraying fluidification.
After measured, the liquefier DE value of acquisition is 26.3, contents on dry basis 51.2wt%；Protein flocculates and swims in
On liquefier.It is filtered with No. 101 150mm diameter filter paper, the rate of filtration is that every 4min filters out 39mL.
Embodiment 3:
(1) using commercially available cornstarch as raw material, it is 45wt%'s that butt quality score is prepared in 50 DEG C of tank of sizing mixing
PH is adjusted to 6.0 with 8M hydrochloric acid by starch milk, in terms of starch on dry basis, Xiang Suoshu size mixing be added in tank 0.35 ‰ medium temperature α-shallow lake
Powder enzyme, 0.25 ‰ Thermostable α-Amylase, 0.08 ‰ lipase and 0.12 ‰ neutral proteinase, at 55 DEG C after mixing
1.5h is kept the temperature, the first starch milk that brix value is 17% is obtained；
(2) cornstarch is added in stirring in the first starch milk of Xiang Suoshu, obtains second that butt quality score is 70wt%
Starch milk, Xiang Suoshu sizes mixing, and 0.35 ‰ mesophilicα-diastase, 0.25 ‰ Thermostable α-Amylase, 0.08 ‰ are added in tank
Lipase and 0.12 ‰ neutral proteinase obtain the third that brix value is 22% in 55 DEG C of heat preservation 0.5h or more after mixing
Starch milk；
(3) with 0.18m3The third starch milk is carried out injection liquefaction through pipeline discharge by/h, and the temperature of jet port is
It 108 DEG C and maintains in pipe 3 minutes, steam pressure 0.6MPa.The injection liquefaction products are flashed, temperature is dropped
To 98 DEG C, 2h then is kept the temperature at 95 DEG C, obtains liquefier；While spraying liquefaction, with the speed of 85kg/h to the tune
Water is supplemented in slurry tank；Cornstarch is supplemented into the tank of sizing mixing with the speed of 114.8kg/h, so that object in the tank of sizing mixing
The butt quality score of material is 70wt%, while supplementing 0.35 ‰ mesophilicα-diastase, 0.25 ‰ high temperature resistant alphalise starch
Enzyme, 0.08 ‰ lipase and 0.12 ‰ neutral proteinase (in terms of starch on dry basis) realize consecutive spraying fluidification.
After measured, the liquefier DE value of acquisition is 25.7, contents on dry basis 66.3wt%；Protein flocculates and swims in
On liquefier.It is filtered with No. 101 150mm diameter filter paper, the rate of filtration is that every 4min filters out 18mL.
Embodiment 4
(1) to dry cornstarch as raw material, it is 40wt%'s that butt quality score is prepared in 50 DEG C of tank of sizing mixing
PH is adjusted to 6.0 with 8M hydrochloric acid by starch milk.In terms of starch on dry basis, Xiang Suoshu size mixing be added in tank 0.2 ‰ medium temperature α-shallow lake
Powder enzyme, 0.2 ‰ Thermostable α-Amylase, 0.08 ‰ lipase and 0.12 ‰ neutral proteinase, after mixing 55 DEG C protect
Warm 0.5h obtains the first starch milk that brix value is 13%；
(2) with 0.18m3First starch milk is carried out injection liquefaction through pipeline discharge by/h, and the temperature of jet port is
It 108 DEG C and maintains in pipe 3 minutes, steam pressure 0.6MPa.The injection liquefaction products are flashed, temperature is dropped
To 98 DEG C, 2h then is kept the temperature at 95 DEG C, obtains liquefier.
After measured, the liquefier DE value of acquisition is 22.5, and protein coagulation is obvious, swims on liquefier.With
No. 101 150mm diameter filter paper filterings, the rate of filtration are that every 4min filters out 47mL.
Comparative example 1:
(1) using commercially available cornstarch as raw material, it is 45wt%'s that butt quality score is prepared in 50 DEG C of tank of sizing mixing
PH is adjusted to 6.0 with 8M hydrochloric acid by starch milk, and in terms of starch on dry basis, Xiang Suoshu sizes mixing, and the medium temperature of addition 0.15 ‰ is added in tank
Alpha-amylase and 0.2 ‰ Thermostable α-Amylase, in 55 DEG C of heat preservation 1h after mixing, obtain that brix value is 13% first is formed sediment
Powder cream；
(2) with 0.18m3First starch milk is carried out injection liquefaction through pipeline discharge by/h, and the temperature of jet port is
It 108 DEG C and maintains in pipe 3 minutes, steam pressure 0.6MPa.The injection liquefaction products are flashed, temperature is dropped
To 98 DEG C, 2h then is kept the temperature at 95 DEG C, obtains liquefier.
After measured, the liquefier DE value of acquisition is 20.7.It is filtered with No. 101 150mm diameter filter paper, the rate of filtration is every
4min filters out 20mL.
Comparative example 2:
For comparative example 1,0.15 ‰ mesophilicα-diastase, 0.2 ‰ Thermostable α-Amylase and 0.04 ‰ are only added
Lipase, carry out the step identical as comparative example 1.
After measured, the liquefier DE value of acquisition is 23.7.It is filtered with No. 101 150mm diameter filter paper, the rate of filtration is every
4min filters out 28mL.
Comparative example 3:
For comparative example 1,0.15 ‰ mesophilicα-diastase, 0.2 ‰ Thermostable α-Amylase and 0.07 ‰ are only added
Neutral proteinase, carry out the step identical as comparative example 1.
After measured, the liquefier DE value of acquisition is 22.4.It is filtered with No. 101 150mm diameter filter paper, the rate of filtration is every
4min filters out 42mL.
Measure example: starch milk viscosimetric analysis
The starch milk for taking 30g to be determined pours into the sample jar of RVA viscosity analyser, and setting program is as follows: at 60 DEG C
1.5min is kept the temperature, 95 DEG C is then raised temperature to, is 6min the time required to heating, 5.5min is kept the temperature at 95 DEG C, is then cooled to 50
DEG C, it is 2.5min the time required to cooling, revolving speed is set as 250rpm, measures the viscosity of liquefaction process.To embodiment 1 and comparison
For the viscosity measurements of first starch milk of example 1,2,3 as shown in Figure 1, wherein a curve is blank control group, b curve is pair
1 samples taken viscograph of ratio, c curve are 2 samples taken viscograph of comparative example, and d curve is 3 samples taken of comparative example
Viscograph, e curve are embodiment 1.
The results show that sample after four kinds of enzyme pretreatments, liquefies when 5min, starch milk reaches maximum viscosity, comparison
A, e curve, peak viscosity are reduced to 4440cP from 14080cP, reduce amplitude up to 68.4%；Liquefy 7.5min to 13min, e
Curve is far below a curve, and high viscosity state decreased duration, starch milk viscosity range of decrease effect is fairly obvious when high temperature, viscosity reduction
Effect reaches continuous liquefaction condition.
Claims (14)
1. a kind of preprocess method for promoting high concentration starch liquefacation, the method comprises the following steps: with the shallow lake of 38-55wt%
As substrate mesophilicα-diastase, Thermostable α-Amylase, lipase and neutral proteinase is added, in 45-55 after mixing in powder cream
DEG C heat preservation；
Wherein, the mesophilicα-diastase, the Thermostable α-Amylase, the lipase and the neutral proteinase are with as follows
Ratio be added: in terms of starch on dry basis, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ high temperature resistant alphalise starch
The neutral proteinase of enzyme, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰.
2. a kind of method using steam direct heating liquefaction high concentration starch, the method comprise the steps that
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0, in addition
Warm alpha-amylase, Thermostable α-Amylase, lipase and neutral proteinase are kept the temperature after mixing at 45-55 DEG C, and obtaining brix value is
The first starch milk of 9-18%；
(2) first starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is flashed, it will be warm
Degree is down to 97-99 DEG C, then keeps the temperature 0.5h-3h at 95-97 DEG C, obtains liquefier；Wherein, in the injection liquefaction, injection
The temperature of mouth is 100-110 DEG C, steam pressure 0.5-0.7MPa；
Wherein, the mesophilicα-diastase, the Thermostable α-Amylase, the lipase and the neutral proteinase are with as follows
Ratio be added: in terms of starch on dry basis, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ high temperature resistant alphalise starch
The neutral proteinase of enzyme, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰.
3. method according to claim 2, wherein in step (1), the preparation of starch milk 45-60 DEG C at a temperature of carry out.
4. a kind of method for the high concentration starch that continuously liquefied using steam direct heating, the method comprise the steps that
(1) starch milk that butt quality score is 38-55wt% is prepared in tank of sizing mixing, and pH is adjusted to 5.0-6.0, in addition
Warm alpha-amylase, Thermostable α-Amylase, lipase and neutral proteinase are kept the temperature after mixing at 45-55 DEG C, and obtaining brix value is
The first starch milk of 9-18%；
(2) starch that butt quality score > 70% is added is stirred in the first starch milk of Xiang Suoshu, obtaining butt quality score is
Mesophilicα-diastase, Thermostable α-Amylase, fat are added in the second starch milk of Xiang Suoshu for the second starch milk of 50-70wt%
Enzyme and neutral proteinase obtain the third starch milk that brix value is 10%-24% in 50-60 DEG C of heat preservation 0.5h or more after mixing；
And
(3) the third starch milk is subjected to injection liquefaction through pipeline discharge, the injection liquefaction products is flashed, it will be warm
Degree is down to 97-99 DEG C, then keeps the temperature 0.5h-3h at 95-97 DEG C, obtains liquefier；While injection liquefaction, to institute
State starch, water and mesophilicα-diastase, Thermostable α-Amylase, the fat that butt quality score > 70% is supplemented in tank of sizing mixing
Enzyme and neutral proteinase；Wherein, in the injection liquefaction, the temperature of jet port is 100-110 DEG C, steam pressure 0.5-
0.7MPa；Wherein, the starch and water supplemented makes the butt quality score of material in the tank of sizing mixing be 50-70wt%；
Wherein, in step (1), the mesophilicα-diastase, the Thermostable α-Amylase, the lipase and the neutral egg
White enzyme is added by following ratio: in terms of starch on dry basis, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ resistance to height
The neutral proteinase of warm alpha-amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰.
5. method as claimed in claim 4, wherein in step (1), the preparation of starch milk 45-60 DEG C at a temperature of carry out.
6. method as claimed in claim 4, wherein in step (2), the mesophilicα-diastase, the high temperature resistant alphalise starch
Enzyme, the lipase and the neutral proteinase are added with following ratio to second starch milk: with second starch
Starch on dry basis meter in cream, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase,
0.04 ‰ -0.08 ‰ lipase and the neutral proteinase of 0.07-0.12 ‰.
7. method as claimed in claim 4, wherein in step (3), with 0.1-0.2m3The speed of/h pumps third starch milk.
8. method as claimed in claim 4, wherein in step (3), supplemented with the speed of 110-120kg/h into tank of sizing mixing
Starch.
9. method as claimed in claim 4, wherein in step (3), supplement water into tank of sizing mixing with the speed of 80-90kg/h.
10. method as claimed in claim 4, wherein in step (3), the mesophilicα-diastase, the high temperature resistant alphalise starch
Enzyme, the lipase and the neutral proteinase are added with following ratio to the tank of sizing mixing: with the dry of the starch that is supplemented
Base meter, 0.1 ‰ -0.4 ‰ mesophilicα-diastase, 0.2 ‰ -0.3 ‰ Thermostable α-Amylase, 0.04-0.08 ‰ fat
The neutral proteinase of enzyme and 0.07-0.12 ‰.
11. method as claimed in claim 4, described method includes following steps:
(1) starch milk that butt quality score is 38-55wt% is prepared in 50 DEG C of tank of sizing mixing, pH is adjusted to 6.0, to form sediment
Dried bean noodles base meter, Xiang Suoshu size mixing mesophilicα-diastase, 0.2-0.3 ‰ that 0.1-0.4 ‰ is added in tank Thermostable α-Amylase,
The lipase of 0.04-0.08 ‰ and the neutral proteinase of 0.07-0.12 ‰ obtain brix in 55 DEG C of heat preservation 0.5-1h after mixing
Value is the first starch milk of 9%-18%；
(2) starch that butt quality score > 70% is added is stirred in the first starch milk of Xiang Suoshu, obtaining butt quality score is
The second starch milk of 50-70wt%, Xiang Suoshu size mixing the resistance to of the mesophilicα-diastase, 0.2-0.3 ‰ that 0.1-0.4 ‰ is added in tank
The neutral proteinase of high-temperatureα-amylase, the lipase of 0.04-0.08 ‰ and 0.07-0.12 ‰ is kept the temperature after mixing at 55 DEG C
0.5h or more obtains the third starch milk that brix value is 10%-24%；And
(3) with 0.1-0.2m3The third starch milk is carried out injection liquefaction through pipeline discharge by/h, to the injection liquefaction products
It is flashed, cools the temperature to 97-99 DEG C, then kept the temperature 1h-3h at 95-97 DEG C, obtain liquefier；It liquefies in the injection
While, Xiang Suoshu, which sizes mixing, supplements starch, water and mesophilicα-diastase, the high temperature resistant α-of butt quality score > 70% in tank
Amylase, lipase and neutral proteinase；Wherein, in the injection liquefaction, the temperature of jet port is 100-110 DEG C, vapour pressure
Power is 0.5-0.7MPa；Wherein, starch is supplemented into tank of sizing mixing with the speed of 110-120kg/h, and with the speed of 80-90kg/h
Water is supplemented into tank of sizing mixing, so that the starch and water that are supplemented make the butt quality score of material in the tank of sizing mixing be 50-
70wt%；Wherein, mesophilicα-diastase, Thermostable α-Amylase, lipase and the neutral proteinase supplemented are as follows: to be supplemented
Starch on dry basis meter, the mesophilicα-diastase of 0.1-0.4 ‰, the Thermostable α-Amylase of 0.2-0.3 ‰, 0.04-0.08 ‰
The neutral proteinase of lipase and 0.07-0.12 ‰.
12. such as method of any of claims 1-11, wherein DE value of the liquefier with 22-28 and
The dry matter content of 40wt%-70wt%.
13. method according to claim 1 or 2, wherein prepare starch milk to dry cornstarch as raw material.
14. method as claimed in claim 13, wherein in step (1), it is 38- that butt quality score is prepared in tank of sizing mixing
The starch milk of 50wt%.
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