CN104911235A - Medical dextrose monohydrate production technology - Google Patents
Medical dextrose monohydrate production technology Download PDFInfo
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- CN104911235A CN104911235A CN201510267883.7A CN201510267883A CN104911235A CN 104911235 A CN104911235 A CN 104911235A CN 201510267883 A CN201510267883 A CN 201510267883A CN 104911235 A CN104911235 A CN 104911235A
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Abstract
The invention belongs to the field of dextrose processing technologies and particularly relates to a medical dextrose monohydrate production technology. The medical dextrose monohydrate production technology includes the steps of liquidation, saccharification, impurity removing, concentration, decoloration, crystal separation, drying and the like. Compared with the prior art, the medical dextrose monohydrate production technology has the advantages that through changing the traditional technology and utilizing the technical means such as secondary injection, high-purity medical dextrose monohydrate is reasonably prepared from corn starch milk, the amount of enzymes added in the whole technology is small, the technology is simple, and the utilization rate of the corn starch milk is high; novel equipment is added into the technology, resources are effectively reused, and therefore the purposes of energy conservation and environmental friendliness are achieved.
Description
Technical field
The invention belongs to glucose complete processing field, particularly relate to a kind of medicinal DEXTROSE MONOHYDRATE BP production technique.
Background technology
Glucose is also called corn sugar, corn sugar, and even referred to as glucose, be the widest and of paramount importance a kind of monose of distributed in nature, it is a kind of poly-hydroxy aldehyde.Pure glucose is clear crystal, and pleasantly sweet but sweet taste, should be water-soluble not as sucrose, is slightly soluble in ethanol, is insoluble to ether.Aqueous solution optically-active to the right, therefore also known as " dextrose ".Glucose has critical role in field of biology, is the energy derive of viable cell and metabolic intermediate product.Meanwhile, glucose is in candy making industry and field of medicaments extensive application.
Crystalline dextrose can be divided into DEXTROSE MONOHYDRATE BP (C according to the difference of manufacturing process
6h
12o
6.H
2and dextrose anhydrous (C O)
6h
12o
6).One water crystallization glucose is divided into food grade glucose and medical glucose, and food grade glucose is mainly used in food-processing industry and fresh-keeping of vegetables industry.DEXTROSE MONOHYDRATE BP can manufacture sorbyl alcohol through hydrogenation, and pharmaceutical grade DEXTROSE MONOHYDRATE BP is mainly expected as former (auxiliary) of oral pharmaceutical.
In order to the purity of the output and glucose that improve DEXTROSE MONOHYDRATE BP, there has been proposed various scheme, such as State Intellectual property right document provides a kind of method for making [application number: 86106624.3] of crystalline glucose for medicine, the method of this invention uses debranching factor and glucoamylase and starch hydrolyzates effect, obtain the high purity liquid glucose of more than content glucose 97% purity, liquid glucose is exquisite, concentrated again, just can obtain crystalline dextrose.
Although aforesaid method improves the output of DEXTROSE MONOHYDRATE BP and the purity of glucose to a certain extent, but it in process of production, need a large amount of debranching factors and glucoamylase, thus improve production cost, in addition, use the method, easily produce a large amount of waste liquids, easily cause the pollution of environment and the waste of resource.
Summary of the invention
The present invention is directed to above-mentioned medicinal glucose production method and there is a large amount of waste liquid of high, the easy generation of production cost, thus cause the technical problems such as the pollution of environment, propose a kind of reasonable in design, preparation time is short, production cost is low and the medicinal DEXTROSE MONOHYDRATE BP production technique that waste liquid amount is few.
In order to achieve the above object, the technical solution used in the present invention is, the invention provides a kind of medicinal DEXTROSE MONOHYDRATE BP production technique, comprises step:
A, liquefaction: adopt second spraying technique to carry out liquefaction processing to corn starch milk, concrete steps are in material-compound tank, add corn starch milk and be equivalent to the α-amylase of corn starch milk 1/3 volume simultaneously, to heat in adding procedure enzyme, heat to 110 DEG C and maintain 1 minute;
B, after h step terminates, then by the Liquid transfer in material-compound tank to maintenance tank in flash distillation cool to 95 DEG C and maintain 20 minutes;
C, then by the Liquid transfer that maintains in tank in vapor can, then be warmed up to 135 DEG C by steam heating and maintain 15 seconds;
D, after j step terminates, by in the Liquid transfer in vapor can tank to liquefied pot and flash distillation cool to 93 DEG C, carry injection simultaneously in the process of cooling to add the α-amylase being equivalent to corn starch milk 2/3 volume in a step again and carry out enzyme, in liquefied pot, temperature maintains 93 DEG C and 90 minutes, after end, obtain the W-Gum liquid glucose of post liquefaction DE value between 12 ~ 14.
E, saccharification: add saccharifying enzyme in W-Gum liquid glucose Step d obtained, carry out saccharification react, obtain saccharified liquid;
F, decon: utilize rotary drum filtration, activated carbon decolorizing filters and ion-exchange three kinds of technique means remove various insoluble impurities and soluble impurity in saccharified liquid;
G, enrichment step are mainly divided into pre-concentration process and reconcentration process, and wherein pre-concentration process is: utilize MVR vaporizer that saccharified liquid is concentrated into concentration about 50%;
H, reconcentration process: saccharified liquid pre-concentration being obtained about 50% concentration is transported to triple effect waste heat evaporator and carries out reconcentration, obtain the dense syrup that concentration is 68%-72%;
I, decolouring: use gac to be dense syrup decolorization process, obtain the dense syrup after decolouring;
J, first to stir in the dense syrup delivery surge tank decoloured;
K, by the dense syrup delivery that stirred in crystallizer, add crystal seed simultaneously and mix.
After l, naturally cooling 12h, obtain the massecuite of advantages of good crystallization, then by the massecuite of advantages of good crystallization input whizzer, carry out centrifugation, obtain water-containing crystal glucose and remaining dense syrup;
M, remaining dense syrup to be added in crystallizer again, to repeat k step and l step, obtain dextrose hydrate crystallization;
N, drying: by dextrose hydrate crystallization by drying unit drying obtain water ratio lower than 9% DEXTROSE MONOHYDRATE BP crystal.
As preferably, described whizzer is top-suspended basket centrifuge
As preferably, drying unit is the fixed fluidized bed drying unit of round shape back-mixing bed adverse current.
As preferably, the fixed fluidized bed drying unit of described round shape back-mixing bed adverse current comprises fixed fluidized bed drying machine, Vibratingfluidbeddrier and vibrated fluidized bed cooler.
Compared with prior art, advantage of the present invention and positively effect are,
1, the present invention is by changing traditional technique, and utilize the technique means such as second spraying technique, reasonably obtain highly purified medicinal DEXTROSE MONOHYDRATE BP from W-Gum Ruzhong, in whole technique, enzyme concentration is few, and technique is simple, corn starch milk utilization ratio is high.
2, the present invention goes by being added in technique by novel equipment, effectively resource is reused, thus reaches the object of energy-saving and environmental protection.
Embodiment
In order to more clearly understand above-mentioned purpose of the present invention, feature and advantage, below in conjunction with specific embodiment, the present invention will be further described.It should be noted that, when not conflicting, the feature in the embodiment of the application and embodiment can combine mutually.
Set forth a lot of detail in the following description so that fully understand the present invention, but the present invention can also adopt and be different from other modes described here and implement, and therefore, the present invention is not limited to the restriction of the specific embodiment of prospectus below.
Embodiment 1, first simultaneously in material-compound tank, add corn starch milk and be equivalent to add the α-amylase of corn starch milk 1/3 volume, in adding procedure, material-compound tank will progressively heat up, when being warming up to 110 DEG C, keep this temperature and maintain 1 minute (fully mixing with α-amylase to make W-Gum, when adding, the flow of corn starch milk and α-amylase should be controlled, find through lot of experiments, the flow of corn starch milk remains on 99169Kg/h, the flow of α-amylase remain on 5.0L/h can make corn starch milk and α-amylase abundant, consider that the activity of normal enzyme reduces along with the rising of temperature, and the decline of enzyme activity can bring the harm of two aspects, one is affect hydrolysis effect, the consumption increasing enzyme in production again, therefore use high temperature resistant α-amylase in the present embodiment),
Then by the liquid in material-compound tank by pump delivery to maintenance tank in and utilize air-cooler flash distillation to cool to 95 DEG C and maintain 20 minutes; Again by the Liquid transfer that maintains in tank in vapor can, then be warmed up to 135 DEG C by steam heating and maintain 15 seconds;
After above-mentioned steps terminates, by in the Liquid transfer in vapor can tank to liquefied pot and flash distillation cool to 93 DEG C, carry injection simultaneously in the process of cooling to add the α-amylase being equivalent to add at first corn starch milk 2/3 volume again and carry out enzyme, in liquefied pot, temperature maintains 93 DEG C and 90 minutes, after end, obtain W-Gum liquid glucose, the DE value of the W-Gum liquid glucose at this time obtained is between 12 ~ 14.
DE value is too high, and one is can directly produce at liquefaction stage the ultrashort chain molecular saccharides be much difficult to by Glucoamylase hydrolysis, such as maltose and trisaccharide maltose, finally affects the DX value of saccharified liquid.Two is that average mark subchain is too short, more difficult with the combination of saccharifying enzyme, can extend the consumption of saccharification time or increase saccharifying enzyme on the contrary; DE value is too low, and the viscosity of W-Gum liquid glucose is comparatively large, also can increase the difficulty of saccharification.
To obtain W-Gum liquid glucose is transported in saccharifying tank, adds saccharifying enzyme simultaneously, and the amount of putting into of saccharifying enzyme is answered, and add by the amount of every gram of starch milk 20U, and holding temperature is at 60 DEG C, pH value is 4.5, and stirring reaction 60h, finally obtains saccharified liquid.
Due in the saccharified liquid that obtains containing a large amount of non-carbohydrate impurity, these impurity can be divided into the water-insoluble impurity based on protein, the dissolved organic matter impurity based on pigment and inorganic salts solubility ashy substance according to property sort.
In the present embodiment, adopt vacuum drum to filter for the water-insoluble impurity based on protein and remove, main process is vacuum drum first will hang up one deck 12 ~ 15cm before filter material super-cell on the surface of rotary drum, is commonly called as and hangs soil.Start filter material under the promotion of pull of vacuum after, the filter cake being attached to diatomite surface, with the slow feed of speed of about 1cm per hour, scrapes by scraper at any time.Certainly, diatomite layer is also scraped off very thin one deck simultaneously.When diatomite layer is left to only have 2 ~ 3cm, stop charging, material has filtered rear manual feed and has been scraped completely on diatomite surface totally, and just can mend (extension) soil by the caliper recovery of diatomite layer to 12 ~ 15cm, like this circulation carries out the continuous filtration of liquid glucose.
For the dissolved organic matter impurity based on pigment, the mode that the present embodiment mainly adopts activated carbon decolorizing to filter, key step, for using plate basket Filter Press, is filtered finally by 0.5 micron of accurate filter inspection.Because of after saccharified liquid decolorization filtering not again through ion-exchange, so gac used must use pharmaceutical grade charcoal, preferably wash charcoal with water.
Adopt the mode of ion-exchange for inorganic salts solubility ashy substance, key step is that saccharified liquid enters ion-exchange pond, adsorbs inorganic salts solubility ashy substance by resin.
Preconcentration steps adopts MVR vaporizer, and equipment is provided by Shanghai Xuan Ke company the whole series, and the vaporization temperature of MVR vaporizer is lower, and because MVR vaporizer adopts single-effect vacuum evaporation, vaporization temperature is equivalent to the end effect vaporization temperature of multiple-effect falling film vaporizer.The low concentrated very good saccharified liquid to saccharified liquid of vaporization temperature is not deepened substantially in concentration process color.In the present embodiment, saccharified liquid is concentrated into concentration 50%.
When it should be noted that MVR vaporizer for concentrated saccharified liquid, discharge concentration is no more than 55%, because the elevation of boiling point of 55% concentration liquid glucose has reached more than 3 DEG C, the elevation of boiling point is larger, and effective heat transfer temperature difference of evaporation is less.More than 55% sugar concentration continues to rise, and the elevation of boiling point accelerates to rise, and the steam output of MVR vaporizer will decline fast.
Consider the characteristic of MVR vaporizer, therefore must first vacuumize before startup MVR vaporizer, MVR vaporizer runs when vacuum degree deficiency, and its power consumption can rise fast and cause motor to trip, even motor damage time serious.Should also be noted that the motor of MVR vaporizer must not the operation more than 50 hertz, otherwise occur same problem.
Ensuing reconcentration step needs by MVR vaporizer pre-concentration to concentration about 50%, then sends to triple effect waste heat evaporator and be concentrated to crystallization desired concn further.The steam flashed off in liquefying starch breast process before triple effect waste heat evaporator uses is thermal source, and its temperature is about 90 ~ 93 DEG C, and after reconcentration step terminates, will obtain concentration is the dense syrup of 68-72%.
Decolorization process is the procedure added in order to ensure the finished product, its need add gac very low, be about amount of dry matter ten thousand/to very much son three.The useless charcoal that dense syrup decolorization produces still has certain decolorizing ability, if can ensure fresh change, can continue to use.
After dense syrup decolorization is completed, next be exactly the step of Crystallization Separation, Crystallization Separation step mainly adopts secondary grading crystallization processes in the present embodiment, first be that the 68-72% dense syrup pump that decolours is squeezed in the first surge tank with the flow velocity of 36385kg/h by concentration, after stirring lower blade in dense syrup submergence first surge tank, start the agitator in the first surge tank and set temperature is 96 DEG C, when liquid level reaches 60% of the first surge tank, opening the first surge tank outlet valve and arranging flow is 25m
3/ h, after being filtered, syrup delivery enters in the second surge tank by ejector priming, after stirring lower blade in dense syrup submergence second surge tank, start agitator in the second surge tank and set temperature is 53 DEG C, when liquid level reaches the second surge tank 30%, opening the second surge tank outlet valve and arranging flow is 25m
3/ h, after being filtered, dense syrup enters in the 3rd surge tank by ejector priming, after stirring lower blade in dense syrup submergence the 3rd surge tank, start the agitator in the 3rd surge tank and set temperature is 45 DEG C, when liquid level reaches 50%, opening the 3rd surge tank outlet valve and arranging flow is 50m
3/ h, after being filtered, close the first surge tank outlet valve and ejector priming to charging in crystallizer.In combinations kind tank, crystal seed is added with worm conveyor, after the quantity of crystal seed is qualified (in the present embodiment, said quantity is qualified refers to that crystal seed reaches the proportioning with dense syrup, and proportioning is digital known by those skilled in the art, therefore in the present embodiment, no longer mention), with 15m
3/ h flow enters crystallizer, with 45m
3the syrup of/h flow mixes under the effect of crystallizer agitator, and Temperature fall 12 hours, when rate to be crystallized reaches requirement, separates massecuite, and remaining material, adds crystal seed and repeat above-mentioned crystallization processes, reach the object of two-stage crystallization.
Consider that from improving the quality of products crystallization adopts 40 cubes of horizontal decrease temperature crystalline machines.Horizontal crystallizer, compared with the vertical cooling crystallizer of continuous crystallisation, has crystal grain packed uniform and percent crystallization in massecuite (xln dry account for the total dry of massecuite only than) high advantage, adopts the top-suspended basket centrifuge of Guangxi Su Shi group in the present embodiment.
The massecuite of advantages of good crystallization enters whizzer, under the influence of centrifugal force, high-purity crystallized glucose is wherein deposited in the basket of whizzer, still dissolves glucose in the solution and a small amount of assorted sugar is glucose mother liquid (or claiming grape molasses) after whizzer throws away.Glucose mother liquid should make rational arrangement according to its purity.
The moisture crystalline dextrose obtained after Crystallization Separation is mainly sent into the fixed fluidized bed drying machine of round shape back-mixing bed adverse current that pressure is 3.5kpa, temperature is 80 DEG C and (is adopted the method that the present embodiment provides by ensuing drying step, according to strict step, general obtained for water content be the crystalline dextrose of 14%), be characterized in hot blast and the complete counter current contact of material, the moisture of 90-95% can be dried; Send into through the dried crystalline dextrose of fixed fluidized bed drying machine the Vibratingfluidbeddrier that pressure is 350pa, temperature is 43 DEG C, under the effect of vibratory screening apparatus, screen out comprised moisture; Send into normal pressure through the dried crystalline dextrose of Vibratingfluidbeddrier, temperature is the vibrated fluidized bed cooler of 13 DEG C, obtains the finished product through cooling.
In the present embodiment, the temperature provided, pressure and PH scope all record through many experiments, and when specifically using, temperature range deviation ± 5 DEG C, pressure divergence ± 100pa, pH value deviation ± 0.5 all should be the claimed content of the present invention.
Detect: detect according to standards of pharmacopoeia for the medicinal DEXTROSE MONOHYDRATE BP using present method to produce
Through inspection, the medicinal DEXTROSE MONOHYDRATE BP using present method to produce meets state-promulgated pharmacopoeia standard, and is better than the medicinal DEXTROSE MONOHYDRATE BP of produced in conventional processes.
The above; it is only preferred embodiment of the present invention; it is not restriction the present invention being made to other form; the Equivalent embodiments that any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as equivalent variations is applied to other field; but everyly do not depart from technical solution of the present invention content; according to any simple modification, equivalent variations and remodeling that technical spirit of the present invention is done above embodiment, still belong to the protection domain of technical solution of the present invention.
Claims (10)
1. a medicinal DEXTROSE MONOHYDRATE BP production technique, is characterized in that, comprise the following steps:
A, liquefaction: use second spraying technique to be liquefied by corn starch milk, obtain the W-Gum liquid glucose of post liquefaction DE value between 12 ~ 14;
B, saccharification: add saccharifying enzyme in W-Gum liquid glucose a step obtained, carry out saccharification react, obtain saccharified liquid;
C, decon: remove various insoluble impurities and soluble impurity in saccharified liquid;
D, concentrated: concentrated by the saccharified liquid after removing impurity, concentrated concentration, to 68%-72%, obtains dense syrup;
E, decolouring: use gac to be dense syrup decolorization process, obtain the dense syrup after decolouring;
F, Crystallization Separation: adopt secondary crystallization process that the dense syrup processing after decolouring is obtained dextrose hydrate crystallization;
G, drying: by dextrose hydrate crystallization by drying unit drying obtain water ratio lower than 9% DEXTROSE MONOHYDRATE BP crystal.
2. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 1, is characterized in that, described second spraying technique comprises following concrete steps:
H, while, add corn starch milk and be equivalent to the α-amylase of corn starch milk 1/3 volume, enzyme of heating in adding procedure in material-compound tank, heats to 110 DEG C and maintain 1 minute;
I, after h step terminates, then by the Liquid transfer in material-compound tank to maintenance tank in flash distillation cool to 95 DEG C and maintain 20 minutes;
J, then by the Liquid transfer that maintains in tank in vapor can, then be warmed up to 135 DEG C by steam heating and maintain 15 seconds;
K, after j step terminates, by in the Liquid transfer in vapor can tank to liquefied pot and flash distillation cool to 93 DEG C, carry injection simultaneously in the process of cooling to add the α-amylase being equivalent to corn starch milk 2/3 volume in h step again and carry out enzyme, in liquefied pot, temperature maintains 93 DEG C and 90 minutes, after end, obtain the W-Gum liquid glucose of post liquefaction DE value between 12 ~ 14.
3. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 1, it is characterized in that, described step c mainly utilizes the technique means such as rotary drum filtration, activated carbon decolorizing filtration and ion-exchange to remove various insoluble impurities and soluble impurity in saccharified liquid.
4. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 1, is characterized in that, described Step d comprises pre-concentration process and reconcentration process.
5. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 4, is characterized in that, saccharified liquid is concentrated into concentration about 50% for utilizing MVR vaporizer by described pre-concentration process.
6. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 4, it is characterized in that, described reconcentration process is that starch saccharificating liquid pre-concentration being obtained about 50% concentration is transported to triple effect waste heat evaporator and carries out reconcentration, obtains the dense syrup that concentration is 68%-72%.
7. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 1, it is characterized in that, described secondary crystallization process comprises following concrete steps:
L, first to stir in the dense syrup delivery surge tank decoloured;
M, by the dense syrup delivery that stirred in crystallizer, add crystal seed simultaneously and mix.
After n, naturally cooling 12h, obtain the massecuite of advantages of good crystallization, then by the massecuite of advantages of good crystallization input whizzer, carry out centrifugation, obtain water-containing crystal glucose and remaining dense syrup;
O, remaining dense syrup to be added in crystallizer again, Repeated m step and n step.
8. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 7, is characterized in that, described whizzer is top-suspended basket centrifuge.
9. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 1, is characterized in that, the drying unit used in described g step is the fixed fluidized bed drying unit of round shape back-mixing bed adverse current.
10. medicinal DEXTROSE MONOHYDRATE BP production technique according to claim 9, is characterized in that, the fixed fluidized bed drying unit of described round shape back-mixing bed adverse current comprises fixed fluidized bed drying machine, Vibratingfluidbeddrier and vibrated fluidized bed cooler.
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