CN101781665A - Industrialized method for directly producing gluconate by corn flour - Google Patents
Industrialized method for directly producing gluconate by corn flour Download PDFInfo
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- CN101781665A CN101781665A CN 201010134451 CN201010134451A CN101781665A CN 101781665 A CN101781665 A CN 101781665A CN 201010134451 CN201010134451 CN 201010134451 CN 201010134451 A CN201010134451 A CN 201010134451A CN 101781665 A CN101781665 A CN 101781665A
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Abstract
The invention provides a method for directly producing gluconate by corn kernel flour, which comprises the steps of pulping, liquifying and saccharifying. The method is characterized in that corn flour with the grain diameter of 50 to 80 meshes, the water content of no more than 12 percent, the fat content of no more than 0.6 percent and the starch content of no less than 90 percent is used as the raw material in the pulping step. In addition, the invention also relates to the corn flour used for the aim of the invention and a method for producing the corn flour. By adopting the method, the production processes from corn kernels to the gluconate can be reduced, and the cost and the environmental burden are lowered.
Description
Technical field
The present invention relates to the method for suitability for industrialized production gluconate, relate more specifically to produce the method for gluconate by beautiful Semen Maydis powder.
Background technology
The production technology of domestic known gluconic acid product salt mainly contains two kinds at present: a kind of is to be formed by fermentation using bacteria with crystalline dextrose.Another kind is to be made through catalytic oxidation by crystalline dextrose.These two kinds of technological methods are each has something to recommend him, also go back each defectiveness.At first the defective of its coexistence is to be raw material by crystalline dextrose (or ative starch).The starting raw material of producing at present crystalline dextrose is a W-Gum, step such as generally include enzyme liquefaction, enzyme glycolysis, refining, crystallization and separate.Technology is comparatively complicated, and the energy consumption height causes crystalline dextrose with high costs.
This shows that the industrial chain of gluconate is longer at present, need to produce crystalline dextrose by W-Gum again, produce links such as gluconate at last again by crystalline dextrose through producing W-Gum by corn grain.
Therefore, the technology that prior art need be upgraded, to shorten industrial chain, save produce, manpower that material stream passed is brought and the additive decrementation aspect the energy.
Summary of the invention
The present invention aims to provide a kind of coarse raw materials (corn or other starch-containing materials) and directly makes saccharification liquid and directly be used for being converted into the industrial method of gluconate, with the production link that reduces prior art with reduce cost.
In a first aspect of the present invention, a kind of industrial method by directly producing gluconate by corn flour is provided, comprise and size mixing, liquefy and the step of saccharification, it is characterized in that, in the step of sizing mixing, with particle diameter is 50-80 order, moisture content≤12%, fat≤0.6%, and the Semen Maydis powder of starch content 〉=90% is a raw material.
In a second aspect of the present invention, be provided for first aspect purpose Semen Maydis powder.
In a third aspect of the present invention, a kind of method that is used to produce above-mentioned Semen Maydis powder is provided, comprise the step of taking off embryo, abrasive dust and screening, it is characterized in that corn grain was used the water-wet of 0.3-1% weight before taking off embryo, and carried out repeating more than 3 times and take off embryo, and, corn grain reaches required particle diameter through fragmentation repeatedly, sieves after broken, to remove the slag ingredient of non-starch at every turn.
Adopt method of the present invention, prepare starch with of the prior art by corn, prepare crystalline dextrose by starch again, a plurality of production links that prepare gluconate by crystalline dextrose are simplified greatly again, both improve production efficiency, reduced energy consumption and environmental pressure again.
Embodiment
The method for preparing gluconate by corn that relates among the present invention comprises three phases generally: powder process, promptly make the Semen Maydis powder that suits the requirements by corn grain; Saccharification changes into glucose with Semen Maydis powder; And follow-up hydrochlorateization, with the gluconic acid of glucose oxidase one-tenth.Below the various embodiments in each stage of the inventive method are described in detail.
One, powder process
For the needs of subsequent step of the present invention, be used for Semen Maydis powder of the present invention and must reach following requirement: all particle diameters are about 60 orders, and 50-80 order for example is preferably at the 60-80 order; Moisture content≤12%, preferred 12%; Fat≤0.6%, preferred＜0.6%; Starch content 〉=90%, preferred＞90% (doing meter).The Semen Maydis powder that meets these requirements can substitute starch and be directly used in the production gluconate.
In a kind of embodiment of the present invention, this pulverizing process comprises and takes off embryo, abrasive dust and screening step.
Take off embryo: be used for corn grain water content of the present invention and should not surpass 14%.Can remove the foreign material that are mixed in corn grain before use, for example, sand grains, leaf of Semen Maydis, Stigma Maydis etc.The present invention adopts semidrying to take off embryo and carries embryo repeatedly.So-called semidrying is taken off embryo and was meant that before taking off plumule with the moistening corn distiller's dried grain of a spot of water, water consumption is suitably between the 0.3-1% of corn grain weight.If the water yield surpasses 1%, then be unfavorable for follow-up dry method abrasive dust, if be less than 0.3%, then be unfavorable for taking off embryo.What is called is carried embryo repeatedly and is meant with the corn germ separator corn grain is repeatedly taken off embryo, normally carries out preferred 4 to 5 times 3 to 6 times.Certainly, it also is feasible taking off embryo more frequently.
Take off embryo and repeatedly take off embryo by semidrying, can obtain the extrusion rate of the plumule of corn grain weight 8% weight, far above the embryo rate of taking off of prior art.The plumule of deviating from is far away expensive in corn, can be used to refine Semen Maydis oil.Therefore, of the present inventionly take off the added value that the embryo method has improved byproduct.
Abrasive dust and screening: in the present invention, can not be broken into particle diameter about 60 orders with taking off corn grain disposable powder behind the embryo, because be not easy to from corn, tell the composition (being referred to as the slag composition) outside the starch, for example cutin, robust fibre, maize peel etc. like this.Should reach predetermined particle diameter by repeatedly milling, and after milling, sieve at every turn, to tell Semen Maydis grit wherein.The preferred steel of stone mill and band mill groove that uses grinds ground corn.In the specific embodiment of the present invention, can corn be milled 6-9 time with stone mill or steel mill, sieve after milling, to remove above-mentioned slag composition at every turn.
Utilize aforesaid method, the Semen Maydis powder particle diameter of acquisition is no more than 50 orders, preferably is no more than 60 orders, moisture content≤12%, fat≤0.6%, starch content 〉=90% (doing meter).Under preferred processing condition, can obtain all at the Semen Maydis powder below 60.Be no more than liquefaction and the saccharification speed that 60 purpose Semen Maydis powder are very beneficial for improving Semen Maydis powder with particle diameter.Semen Maydis powder yield 70% (to corn grain), clean plumule yield 8%, plumule purity very high (nothing is adhered to starch milk and cutin), fine powder (particle diameter is less than 80 purpose Semen Maydis powder) yield 10%, fodder meal yield 12%.The plumule that reclaims can be used to extract vegetables oil, and fine powder can be sold to food factory's food prepared therefrom, and this fine powder is mainly starch, but because its particle diameter is too little, makes the filter operation of back be difficult to carry out, and therefore it should be told from Semen Maydis powder; Fodder meal mainly comprises the slag composition, can be used as animal-feed.Adopt above-mentioned working method, increased output, improved economic benefit.Make the cost of acquisition Semen Maydis powder and the purchasing price of corn maintain an equal level.In addition, the Semen Maydis powder that meets These parameters that is obtained can guarantee to extract zein after the liquefaction in sugaring stage, obtains 320 yuan of profits (sour sodium meter per ton) only.
The Semen Maydis powder that aforesaid method obtained can directly pass through saccharification and oxidation and prepare gluconate.
Two, sugaring
The sugaring stage may further comprise the steps: size mixing → enzyme liquefaction → remove slag → enzyme glycolysis → separating out fat → decolouring → ion-exchange.
1. the Semen Maydis powder that above-mentioned steps is obtained of sizing mixing is metered into one for example jar or in the reactor, adds an amount of water, and pH value is adjusted to the active scope of Ye Huamei that is suitable for.In the present invention, especially, adopt hot water to size mixing, to promote the gelatinization of corn steep liquor.The temperature of hot water usually can be at 40-60 ℃, preferably at 45-55 ℃, most preferably between 48-52 ℃.Under this preferred temperature, size mixing, can also prevent that slurries from being infected by milk-acid bacteria.After adding entry, in slurries, introduce Ye Huamei again, under the temperature of suitable enzymic activity, stir then.The Ye Huamei that uses in the prior art all can be used for the present invention.In one embodiment of the invention, select Ye Huamei at once (LiguozymeSupra) for use available from Novozymes Company.The best pH value of this kind of enzyme is 5.3.
2. enzyme liquefaction
In this step, carry out the steam ejection liquefaction first time with Jet liquefier earlier, continue liquefaction with another equipment then.Before charging, earlier Jet liquefier is preheated to 100～115 ℃, preferably be preheated to 108 ℃.Open reflux then and introduce adjusted good Semen Maydis powder slurry, carry out the above-mentioned first time and spray.The pressure of fresh feed pump can maintain about 0.4Mpa, and vapor pressure can be about 0.6Mpa.After spraying for the first time, material enters the laminar flow jar and liquefies continuously.Since the Ye Huamei that uses in the present invention can not be under above-mentioned high temperature long term maintenance, otherwise Ye Huamei is lost activity, in liquefying continuously, make the Semen Maydis powder slurry under the temperature that reduces, keep for some time, be generally 60～90 minutes, starch chain is fully fragmented into the polymerization degree is several to tens oligose, and liquefaction is the temperature at 90～98 ℃ continuously, preferred 93～95 ℃ temperature.In continuous liquefaction process, detect the degree of liquefaction discontinuously with the iodine colour response.The reaction of iodine liquid promptly can be considered normal for red-purple (DE value 14-16).
Another characteristics of the present invention are, after above-mentioned continuous liquefaction, carry out a steam ejection liquefaction process for the second time.With spray for the first time different, this temperature of spraying for the second time between 130-145 ℃, wherein preferred 135-140 ℃.The purpose of carrying out this high temperature liquefaction process is that protein is wherein fully solidified, and albumen mass-energy after solidifying and water layering well are easy to separate in subsequent step like this.
As further preferred, can before this step, carry out a flash distillation (flash distillation) process, with a large amount of steam in the recovery system.
3. remove slag and filter the slurry that is obtained, to tell the slag in the material, the protein that contains vegetable fibre in this slag and solidify.
4. enzyme glycolysis is in this step, and under the effect of saccharifying enzyme, the oligose in the slurry further is degraded, and is converted into monose---glucose.Can use the known saccharifying enzyme of prior art to carry out saccharification, in a preferred embodiment, with the mixing saccharifying enzyme (Dextrozyme Dx 1.5x) of Novozymes Company's production.As preferably, the temperature of saccharification is 61-62 ℃, and PH is 4.3-4.5, and the consumption of enzyme is preferably 0.7 liter of/ton dry.In a kind of preferred mode of the present invention, saccharification temperature is 65 ℃, and this temperature can reduce the pollution of milk-acid bacteria to saccharification liquid.Being apparent that, also is feasible under other temperature, pH value and consumption, and only its saccharification speed can not reach best.
In a typical operational example, this enzyme glycolysis operation is to carry out in a saccharifying tank, liquefier is feeded to prescribed position, when treating that temperature reaches 65 ℃ after being come by the basin pump, regulate PH to prescribed value PH4.3 (regulating) with 4% hydrochloric acid, drop into the saccharifying enzyme of specified amount, drive agitator and stirred 2 hours, measure one time the DE value, carry out record, after this every DE value of censorship in 5 hours, the DE value rises and can comparatively fast may arrive DE90% in 30 hours after the beginning saccharification, then lift velocity is slack-off, arrive at 90% o'clock in the DE value, strengthen detecting, reach (more than 97%) behind the peak value, open again and stir after 20-30 minute, rapidly blowing.
5. lipid content can be above 0.6% usually in the material of separating out fat after saccharification.Under a few cases, because the inaccuracy of the difference of raw material or processing condition control can obtain lipid content and surpass 0.6% Semen Maydis powder.At this moment, can carry out centrifugation by a layering double overflow whizzer (for example Dorr-Oliver merrco Gsu of Britain Dwyer company).
6. decolouring is introduced saccharification liquid in a still or the jar, at 70-95 ℃, and preferred 75-90 ℃, more preferably stirred 20～30 minutes down at 80～85 ℃, separate then and remove gac.This step is in order to remove the foreign pigment in the deglycation liquid, to improve its transmittance.
7. ion-exchange can contain a large amount of negatively charged ion and positively charged ion in the material of aforesaid operations gained, needs spent ion exchange resin to remove, to reduce the specific conductivity of saccharification liquid.For this reason, after with the Zeo-karb decationize, remove negatively charged ion with the anionite-exchange resin exchange again.As a kind of mode that is more preferably, can adopt the mixing column that uniform mixing yin, yang ion exchange resin together is housed to carry out ion-exchange.Yin, yang ion mixing column technology used herein is that prior art is known, and its detailed content is disclosed in for example " Dian Fentang " of tension force Tian Suozhu, and light industry press is among the 216-220.But, because the cause of its complicated operation does not still have commercial application at present at home.The contriver finds, adopts the mixed bed method to carry out ion-exchange, directly prepares the method for gluconic acid for Semen Maydis powder of the present invention, and speed is faster when catalyzed oxidation.
When carrying out ion-exchange, make the liquid glucose ion exchange column of from top to bottom flowing through.Detect the index of effluent liquid, the control electricity is led below 10-μ Ω/cm, and PH5.0-6.0 will regulate the flow velocity of each post, liquid glucose backflow that will be defective when index is not inconsistent.
By mixed bed ion exchange and centrifugation layering double overflow whizzer, thereby obtain the DE value more than 98%, the DP1 value is 90%, protein is 0 substantially, specific conductivity 10, the high-quality saccharification liquid of transmittance 100%, and on highly successional production line, the limit goes out the oxidation of sugared limit, guaranteed the freshness of saccharification liquid, thereby the quality problems (comprising that crystallised sugar is in the fermentation that is caused aspect the storage transportation and storage) that crystalline dextrose of the prior art is caused by yeast fermentation (especially trigonopsis variabilis fermentation) have been overcome in crystallizer, therefore the saccharification liquid of producing according to the inventive method is carried catalyzed oxidation immediately, speed of response obtains beyond thought effect than fast more than 40% with crystalline dextrose.
Clearly, the operation in the above-mentioned saccharification stage needn't strictness be followed said sequence.For example, before enzyme glycolysis also can occur in and remove slag, also can be after separating out fat, and decolouring also can be before separating out fat.In optimal way of the present invention, be according to size mixing → order of enzyme liquefaction → remove slag → enzyme glycolysis → refining → ion-exchange carries out.
So far, can obtain water white Glucose Liquid.This Glucose Liquid can directly carry out next step catalyzed oxidation.
Three, catalyzed oxidation
Next, can adopt the known method for oxidation of prior art that the glucose solution that obtains is direct oxidation into the gluconic acid salts solution.Known in the art during the catalyzed oxidation of Glucose Liquid, it adopts palladium catalyst usually.This method is disclosed among the CN1153166 in detail, is adopted by domestic most producers at present.
In aforesaid operations, the method for saccharification and catalyzed oxidation is known in the art, except the optimal way of wherein emphasizing.What be readily appreciated that is, those skilled in the art can also prepare gluconate with other known or unknown saccharification and the method for the catalyzed oxidation Semen Maydis powder that comes to obtain from the present invention.Also can conversion of glucose be become gluconate with fermentation using bacteria method or oxydasis method.
An important innovations point of the present invention is that by special corn flouring technology, the Semen Maydis powder that makes processing obtain can directly carry out liquefaction processing, and the liquid glucose that obtains is directly carried out catalyzed oxidation, has saved the link that is prepared W-Gum by corn.This improvement has very big economy and environmental benefit.Particularly, according to original technology, need to make starch with corn earlier, prepare glucose by W-Gum again, gluconic acid manufacturing enterprise needs glucose water-soluble more again, to obtain saccharification liquid.This is waste water resource not only, has also increased energy consumption greatly, also has certain pollution in addition in the Starch Production.Adopt method of the present invention obviously to overcome these defectives, simultaneously, reduced production cost.
Embodiment
Employing meets the Semen Maydis powder of following quality standard and makes raw material: Semen Maydis powder fineness 60 order all-pass, moisture content 12%, fat 0.6%, starch content 90% (doing meter).Preparation process may further comprise the steps: is the slurries of 30wt% with Semen Maydis powder with 50 ℃ of water furnishing concentration, adds high temperature Ye Huamei at once by the amount of 0.7 liter of/ton dry, and pH value is 5.3.In the continuous liquefaction process of enzyme, the high-temperature injection liquefaction temperature is 105-110 ℃ for the first time, and the time is 16 minutes, keeps liquefaction 60-90 minute in the laminar flow jar, and temperature is 90-95 ℃, DE value 12-16%.The high-temperature injection temperature is 135 ℃ for the second time, and the time is 10 minutes.Enter the enzyme glycolysis operation behind the filter cleaner, condition is, with the saccharifying enzyme Dextrozyme Dx1.5x that Novozymes Company produces, 0.7 liter of/ton dry of consumption, 65 ℃ of temperature, pH value 4.3-4.5, time 48-60 hour, DE value 97-98%.Then, experience is made with extra care (decolouring), mixed bed ion exchange step in turn.With bismuth palladium carbon catalyst catalyzed oxidation liquid glucose, transformation efficiency reaches more than 98%.Tell catalyzer through millipore filtration at last, obtain aqua Sunmorl N 60S product.This aqua through concentrating, operations such as crystallization, centrifugal and drying, be converted into solid phase prod.
Through the foregoing description measuring and calculating, with the Sunmorl N 60S cost that the technology of the present invention is produced, power consumption, the three wastes etc. are listed as follows:
Annotate: water, electricity, vapour consumption and discharge of wastewater all do not comprise sugaring and oxidation, only refer to the raw material aspect.
This shows, the technology of the present invention reduce cost and energy-saving and emission-reduction aspect huge superiority is arranged, with this example calculation,, can reduce cost nearly 100,000,000 yuan if produce 100000 tons of products per year, 1,120 ten thousand degree that economize on electricity are economized on coal 270,000 tons, reduce 350,000 tons of sewage discharges.
Claims (12)
1. method by directly producing gluconate by corn flour, comprise and size mixing, liquefy and the step of saccharification, it is characterized in that, in the step of sizing mixing, with particle diameter is 50-80 order, moisture content≤12%, fat≤0.6%, and the Semen Maydis powder of starch content 〉=90% is a raw material.
2. method according to claim 1 is characterized in that, uses 45-55 ℃ warm water to size mixing.
3. method according to claim 1, wherein, in described saccharifying, comprise for the first time steam ejection liquefaction and steam ejection liquefaction for the second time, described first time steam ejection liquefaction temperature between 100～115 ℃, described second time steam ejection liquefaction temperature between 130～145 ℃.
4. method according to claim 3, wherein, after described second spraying, by the protein that removes by filter the vegetable fibre in the saccharification liquid and solidify.
5. method according to claim 1, wherein, fatty with the centrifugal major part of removing of layering double overflow whizzer after described saccharification.
6. method according to claim 1, wherein, as the final step of sugaring, carry out ion-exchange with yin, yang ion exchange resin mixed bed, make the liquid glucose ion exchange column of from top to bottom flowing through, the electricity of controlling flow fluid is led below 10-μ Ω/cm, and PH is at 5.0-6.0.
7. Semen Maydis powder, particle diameter is the 50-80 order, moisture content≤12%, fat≤0.6%, starch content 〉=90%.
8. Semen Maydis powder according to claim 7, its particle diameter is between the 60-80 order.
9. method that is used for the described Semen Maydis powder of production claim 7, comprise the step of taking off embryo, abrasive dust and screening, it is characterized in that, corn grain was used the water-wet of 0.3-1% weight before taking off embryo, and carry out repeating more than 3 times and take off embryo, and corn grain reaches required particle diameter through fragmentation repeatedly, each broken screening afterwards is to remove the slag ingredient of non-starch.
10. method according to claim 9 wherein, carries out taking off embryo 4-5 time.
11., it is characterized in that corn takes off embryo afterwards through 8 road abrasive dust and screenings according to claim 9 or 10 described methods.
12., it is characterized in that device temperature is no more than 60 ℃ in the corn processed whole process according to claim 9 or 10 described methods.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372049A (en) * | 2013-08-15 | 2015-02-25 | 沈玉现 | Technology for producing fructose-glucose syrup through full dry corn degerming powder production |
| CN104830918A (en) * | 2015-04-07 | 2015-08-12 | 山东西王糖业有限公司 | Novel production method of sodium gluconate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858260A (en) * | 2006-05-30 | 2006-11-08 | 赵佃团 | Processing process for producing cerealose using corn as raw material |
| CN101353681A (en) * | 2008-06-20 | 2009-01-28 | 广州双桥股份有限公司 | Method for preparing nitrogen-containing starch syrup by peeled and degermed maize flour polyzyme method |
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2010
- 2010-03-10 CN CN 201010134451 patent/CN101781665A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858260A (en) * | 2006-05-30 | 2006-11-08 | 赵佃团 | Processing process for producing cerealose using corn as raw material |
| CN101353681A (en) * | 2008-06-20 | 2009-01-28 | 广州双桥股份有限公司 | Method for preparing nitrogen-containing starch syrup by peeled and degermed maize flour polyzyme method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372049A (en) * | 2013-08-15 | 2015-02-25 | 沈玉现 | Technology for producing fructose-glucose syrup through full dry corn degerming powder production |
| CN104830918A (en) * | 2015-04-07 | 2015-08-12 | 山东西王糖业有限公司 | Novel production method of sodium gluconate |
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Application publication date: 20100721 |