CN1025156C - Enzyme liq. fluidized bed granulation technology and apparatus thereof - Google Patents
Enzyme liq. fluidized bed granulation technology and apparatus thereof Download PDFInfo
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- CN1025156C CN1025156C CN 90106855 CN90106855A CN1025156C CN 1025156 C CN1025156 C CN 1025156C CN 90106855 CN90106855 CN 90106855 CN 90106855 A CN90106855 A CN 90106855A CN 1025156 C CN1025156 C CN 1025156C
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Abstract
The present invention belongs to technology of granulating, drying and film coating of enzymes and a device thereof, and relates to new technology of continuously preparing a capsule-type enzyme granule preparation by a concentrated enzyme liquid and a new fluidized bed device corresponding developing continuous operation. The working procedures such as enzyme carrying, granulating, drying, grading, film coating, etc., can be completed in the device at the same time. Enzyme products have the advantages of high yield, convenient regulation and control in the granularity of granules, convenient regulation and control in enzyme activity, good water solubility, high stability and long term storage; the technology does not have dust pollution. The technology and the device can be widely used for aspects such as granulating, drying, packing and coating, etc., in industry of chemical industry, metallurgy, medicine, fodder and biochemistry preparation.
Description
The invention belongs to granulation, the drying of enzyme, the technology and the equipment of the aspect of filming, is a method of directly directly being produced the granzyme preparation of capsule type by spissated enzymic fermentation liquid continuously.Processes and apparatus of the present invention can be widely used in granulation, the drying of chemical industry, metallurgy, medicine, feed and biochemical preparation, aspect such as film.
Along with the broad development of biotechnology, the application of enzyme in national economy is increasingly extensive, but that enzyme easily disperses inactivation and uses powdery enzyme dust hazard is serious, contaminate environment, and harm workers ' health, so the granulation of enzyme, the coating process of enzyme grain are subjected to extensively paying attention to and research.
The production method of granzyme preparation obtains very big development over nearly 30 years, and the technology of existing production granzyme preparation can be divided into two big classes substantially:
The first kind, the solid hybrid system.The solid concentrates of enzyme (enzyme mud, enzyme powder) mixes the back and granulates with wobbler or extrusion machine with filling agent, binding agent, auxiliary material etc.Representational technology is that extrusion molding is granulated, and promptly produces the basic protein enzyme granulate with this method as Denmark NOVO company, carries out the fluidized-bed coating after the granulation.Domestic this technology pelletizing forming of yet mainly using of China is not filmed but have.This method can continuous production, and product particle is even, but the technological process of production is long, and equipment is many, and efficient is low, and granular size is restricted, and easily local superheating takes place and cause enzyme deactivation, and the enzyme yield is low.
Second class, core particle carries enzyme process.In advance the carrier powder is made particle (core), will be concentrated enzyme liquid, binding agent then and directly be added to carrier core in the heart, representative processes is a fluidized bed process.This method can directly be used enzyme liquid, and processing power is big, periodical operation, and Granularity Distribution is wide, needs to use earlier drum unit simultaneously, preparation such as disk classer or fluidized-bed carrier core particle, the clear and 61-162 as Japanese Patent, 185, United States Patent (USP) 4,689,297.
Fall behind and the low present situation of plant efficiency in the technology that China produces for improving existing granzyme preparation, improve workman's labor condition, reduce the injury of environmental pollution and human body skin, be simultaneously use in the present prior art liquefied bed drying and granulating exist can not operate continuously, problems such as wide, the complex procedures of Granularity Distribution, cost height, the invention provides one efficiently, the enzyme granulate preparation technology and the equipment of high ability.
The present invention is a kind of novel process of producing the granzyme preparation, also develops a kind of new installation efficiently for realizing the present invention of this novel process, can finish drying, granulation, classification simultaneously, several operations of filming, and realizes operate continuously.Because zymin is easy inactivation under comparatively high temps, when particularly moisture content is high, so drying need be carried out at low temperatures.
Granulating process process of the present invention is that water miscible support powder is joined in the granulation liquefied bed continuously by feeder.Air be liquefied gas and warm air be suspension under the effect of swirling eddy, state rotatablely moves; Enzymic fermentation liquid after concentrating or the clay slurries of enzyme and binding agent are transported to through nozzle and also are sprayed onto equably in the granulation fluidized-bed on the support powder that has liquefied in bed, between carrier particles, form " liquid bridge " and adhere to into small core particle, in layer adhere on the surface of core then and grow up, form particle.Under the hot gas flow effect, solvent is evaporated, and particle constantly is dried.The fluidised bed drying temperature is not selected not influence enzyme activity.Fluidizing gas velocity and rotation gas speed is according to grain graininess, and proportion and bed inventory and select make and desire exsiccant enzyme grain material in liquefied bed and be and suspend and the intensive rotating state, the enhance heat transfer mass transfer process, and the promotion particle is grown up; Treat that particle grows up after specified size, under the effect of classification air-flow, classified pipe is automatically discharged and is entered into the fluidized-bed of filming.Coating liquid is squeezed into nozzle with pump and is sprayed onto particle surface through air atomizing, under the liquid gas flow effect of warm air, make the particle after drying, make it and isolated from atmosphere and form thin film, keep active thereby can make enzyme-support particle be able to long storage on the surface of enzyme-support particle.Particle after filming is discharged by discharge gate.
Can regulate gas velocity in the classification pipe in the art production process of the present invention easily as required, control products obtained therefrom globule size.As for as the Sumizyme MP of washing powder additive, as long as the gas velocity in the controlling classification pipe in 4.2-5.2 meter per second scope, can make and be equivalent to washing powder granularity (18～+ 65 order) and account for the granzyme product more than 95%.
The unit of activity size of explained hereafter enzyme granulate product of the present invention is decided on the amount that concentrates enzyme liquid raw material unit of activity and adding binding agent, and the ratio of available change enzyme liquid and binding agent is regulated.As the concentrated enzyme liquid with 8-20 ten thousand unit of activity/milliliters is raw material, and the ratio of binding agent and enzyme liquid is regulated in the 0.10-1.2 scope, can make the granzyme of 1-10 ten thousand unit of activity/grams.
Water-soluble carrier powder of the present invention can be very extensive, as long as enzyme is not had the effect of paying and all can use the favourable or harmless soluble powder of follow-up process, and as NaCl, NaHCO
3, or the like.When preparation washing powder is used the Sumizyme MP grain of additive, can adopt anhydrous sodium sulphate or tripoly phosphate sodium STPP etc., mean particle size 120-150 order adds the stability that a small amount of polyvinylpyrrolidone, gelatin can increase enzyme this moment in the enzyme liquid, add-on is the 0.1-2.0 grams per liter.
The used binding liquid of the present invention has two classes, a class be with the dilution water glass be binding agent pH=10-13, wherein allocate a small amount of maltose into, binding agent viscosity 10-13C.P.; One class is the aqueous solution such as yellow starch gum, starch or yellow starch gum, starch directly dissolved in is made into binding agent to enzyme liquid that viscosity is 40-150C.P..
The used liniment of the present invention can be a fatty acid ester, alkoxyl alcohol, and polyvinyl alcohol etc., when preparation Sumizyme MP grain, the liniment of employing is the water-soluble high-molecular material polyoxyethylene glycol, its molecular weight is 5,000-10,000, consumption is 0.1-0.5%.
For the fluidizing reactor that cooperates process modification of the present invention is made up of the granulation fluidized-bed and the fluidized-bed of filming, make it and the coaxial one that is connected into of the fluidized-bed of filming by the air chamber of granulation fluidized-bed, the classification pipe wherein is installed; The granulation fluidized-bed also can separate with L with the fluidized-bed of filming and cuts down or star is cut down etc. and to be linked to each other.
Fig. 1 is granulation fluidized-bed and the structural representation of filming and being combined into one.
Fig. 2 is mutual for granulation fluidized-bed and the fluidized-bed of filming separate to be cut down or star such as cuts down at the structural representation that links to each other with L.
Fig. 3 is for pneumatic classification pipe in the fluidized-bed and help and be coated with structural representation.
Fig. 4 is for introducing the spin nozzle structural representation of swirling eddy in the granulation fluidized-bed.
Fig. 5 is coated with the structure enlarged diagram for pneumatic classification pipe bottom helps.
Wherein 1, storage grain bucket, screw feeder
2, granulation distribuor of fluidized bed
3, air chamber
4, pneumatic classification pipe
5, product offtake
6, the distribuor of fluidized bed of filming
7, gas inlet
8, nozzle
9, classification gas inlet
10, rotation gas inlet
11, air-heating furnace
12, nozzle
A, granulation fluidized-bed
B, the fluidized-bed of filming
Q, wire netting
R, cone-shaped block
S, taper reducing
Now further specify equipment of the present invention for example in conjunction with the accompanying drawings.
Fluidized bed plant of the present invention is to be combined by the granulation conical fluidized bed (A) and two fluidized-beds of conical fluidized bed (B) of filming, by the air chamber (3) and the fluidized-bed of filming (B) coaxial linking to each other (Fig. 1) below the grid distributor (2) of granulation fluidized-bed (A), in granulation fluidized-bed (A), carrier material portion is from the bed added by screw feeder, nearly grid distributor (2) is evenly distributed with spin nozzle (13) around the top, swirling eddy (10) through preheating tangentially enters bed by jet pipe, thereby the bed material is produced to rotatablely move, at the bed middle part auxiliary spin nozzle is housed also for larger-size fluidized-bed, to strengthen the bed swirling motion, improve granulation efficiency, the enhancing mass and heat transfer process, liquefied gas is then introduced from grid distributor (2) below air chamber (3), make the liquefaction of bed material, grid distributor is a straight hole porous plate, affixed and the opening in pneumatic classification pipe upper end is in grid distributor (2) central authorities, the bottom is stretched in the fluidized-bed of filming (B), enzyme liquid is then squeezed into nozzle (12) with being sprayed at equably behind the air atomizing on the ebullient carrier with pump, the fluidized-bed of filming also is one to have the conical bed of multihole distributor, liquefied gas (7) enters from grid distributor (6) below, nozzle (8) is placed in classification pipe (4) lower end, coating liquid is squeezed into nozzle (8) through being sprayed at behind the air atomizing on the granzyme after enzyme-added with pump, and the back product of filming is discharged from discharge gate (5); The conical bed of filming also can be split up into two independently fluidized-beds with the granulation fluidized-bed, cut down with L between the two or star is cut down link (Fig. 2), the granzyme product that makes from granulation fluidized-bed (A) cuts down by L or star is cut down and directly joined the fluidized-bed of filming (B), coating liquid with pump squeeze into be installed in a top nozzle (8) behind air atomizing in the spirt bed, liquefied gas (7) then enters the bed through grid distributor (6) from the bed bottom, is coated with membrane granule and discharges from discharge gate (5).The granulation liquefied bed and the fluidized-bed of filming separated by L cut down or star is cut down etc. and to be concatenated into one, the fluidized-bed of filming can operate continuously, but also periodical operation can make the operation modification scope wideer.
The pneumatic classification pipe of present device configuration, according to particle than reconditioning classification Guan Zhongqi speed, promptly adjustable product grade, the length-to-diameter ratio L/D of pneumatic classification pipe＞15-20 can be designed to straight tube and also can make the lobster back form.
Classification pipe bottom can be installed one and helped and be coated with structure in the present device, and this structure is formed (Fig. 3) by a cone-shaped block (R) and taper reducing (S), the nozzle of filming (8) be placed on (R) and (S) between, purpose is to improve the particulate homogeneity of filming.
Classification pipe bottom helps and has its outside of uniform hole or groove around the top that is coated with structure and (Q) wrap up with wire netting (40 or 60 order) in the present device, the port area of hole or groove greater than the section 1.5-2.0 of classification pipe doubly, the classification air-flow through the hole or groove enter equably.
The technologic characteristics of the present invention are: flow process is short, equipment is few, carry enzyme, granulation, drying, classification, the whole technological process of filming and in one or two equipment, to finish products obtained therefrom epigranular, sphericity height continuously, granular size can be controlled on demand, the unit of activity height of enzyme is also adjustable, and enzyme stability is good, but prolonged preservation, and can produce compound enzymic preparation, the technology no dust pollution.
The principal feature of the present invention aspect equipment near tangentially introducing granulation, the turning effort of exsiccant swirling eddy (through the air of preheating) generation intensive above the grid distributor, strengthened heat and mass transfer process in fluidized-bed, promoted granulating.Because swirling eddy is not by grid distributor, thereby the pressure-losses is little, saves power, the while has guaranteed that owing to design on the grid distributor has a pneumatic classification pipe product granularity is more even, is provided with to help in classifier inside to be coated with structure, has improved being coated with film uniformity.The liquefaction bed structure of granulating and film is simple, can realize technological process requirement of the present invention in a set of equipment simultaneously continuously.Can make 10 easily with technology of the present invention and equipment, 000-50, the granzyme preparation of filming of 000u/g also can produce 100, the granzyme of 000u/g.
Example one
The carrier powder is an anhydrous sodium sulphate, size-grade distribution (%wt.) (table is seen the literary composition back)
Concentrate enzyme liquid 136,000u/ml, water glass of binder solution v=10C.P., binding agent/enzyme liquid=1: 1.2; The coating liquid polyglycol solution, concentration 2%, coating liquid straying quatity 600ml/hr, fluidized-bed φ 250/ φ 500mm, the high 500mm of cone, the high 1.4m of top cylinder, liquefied gas 20-22M
3/ hr, classification gas speed 4.2-4.6m/s, rotation gas 50-80m
3/ hr, t bed≤50-70 ℃; Can make granularity 18-65 purpose particle＞95%wt, 22Kg/hr, activity 12,700u/g, enzyme yield～85%, half a year, survival rate 95%.
Example two
The carrier powder is an anhydrous sodium sulphate, size-grade distribution (%wt.):
(table is seen the literary composition back)
Concentrated acid enzyme liquid 116,000u/ml; Ratio in 0.25 is dissolved in yellow starch gum and is concentrated in the enzyme liquid, adds gelatin 0.2g/l, v=60C.P., and granulation fluidized-bed φ 100/ φ 250mm, cylindrical shell is high 1.5 meters, liquefied gas 5M
3/ hr, rotation gas 14M '/hr, classification pipe gas speed 5-5.2M.S.T bed≤50-70 ℃; In φ 100/ φ 300 films fluidized-bed, film, the coating liquid polyoxyethylene glycol, concentration 2%, consumption 50ml/Kg enzyme granulate, t be coated with=40 ℃, product granularity 18-65 order grade be 95-98%wt, activity is 20,000-48,000u/g, enzyme yield 〉=95%.
Example three
Carrier and binding agent add a little polyethylene pyrroles gastral cavity trunk with example 2 in enzyme liquid, in φ 250/ φ 500mm fluidized bed granulation device, and liquefied gas 28M
3/ h, rotation gas 80M
3/ h, rotation gas 80M
3/ hr, classification gas speed 4.2-4.6m/s, t bed=42-52 ℃, the condition of filming makes granzyme granularity 18-65 order, 95.5%wt, enzyme yield＞95% with example 1.
Claims (10)
1, a kind of by concentrated enzyme liquid granulate, dry, film and produce the method for granzyme, it is characterized in that making carrier with the water-soluble powder material below mean particle size 100 orders, join in the granulation fluidized-bed, air be fluidized gas and warm air be suspension under the effect of swirling eddy, state rotatablely moves; The binding liquid that concentrates the aqueous solution such as enzyme liquid and water glass, yellow starch gum, starch, gelatin is carried enzyme, granulation, drying continuously on nozzle is sprayed at carrier in the fluidized-bed; Drying temperature is selected with the vigor that does not influence enzyme, and fluidizing gas velocity and rotation gas speed are selected by inventory in grain graininess, proportion and the bed; Automatically control the homogeneity of product particle granularity, the length-to-diameter ratio L/D of classification pipe＞15 with the pneumatic classification pipe; With the air is under the effect of classification air-flow, grow up to the enzyme-support particle of designated size, classified pipe is discharged automatically and is entered into the fluidized-bed of filming, coating liquid is sprayed on the enzyme granulate surface equably via nozzle, under the liquid gas flow effect of warm air, form thin film at particle surface, make the enzyme grain of filming.
2,, it is characterized in that controlling product granularity with regulating the classification air-flow by the described method of claim 1; For Sumizyme MP, as long as the gas velocity 4.2-5.2 meter per second in the controlling classification pipe can make the granzyme product (18 orders～+ 65 orders are greater than 95%) that is equivalent to the washing powder granularity as the washing powder additive.
3, by claim 1,2 described methods, its feature is that also the unit of activity of prepared product can regulate with the ratio that changes enzyme liquid and binding agent, as the concentrated enzyme liquid with 8-20 ten thousand unit of activity/milliliters is raw material, the ratio of binding agent and enzyme liquid is regulated in the 0.10-1.2 scope, can make 1-10 ten thousand units/gram granzymes.
4, by claim 1,2 described methods, it is characterized in that the water-soluble carrier that Sumizyme MP is adopted is anhydrous sodium sulphate or tripoly phosphate sodium STPP, its mean particle size is the 120-150 order, add a small amount of polyvinylpyrrolidone, gelatin to increase the stability of enzyme in dense enzyme liquid, add-on is the 0.1-2.0 grams per liter.
5, by claim 1,2 described methods, it is characterized in that used binding agent has two classes, is binding agent pH=10-13 with water glass, and viscosity is 10-30C.P.; With yellow starch gum or/and starch or/and aqueous gelatin solution is a binding liquid, viscosity is 40-150C.P..
6, by claim 1,2 described methods, it is characterized in that used liniment is the water-soluble high-molecular material polyoxyethylene glycol, its molecular weight is 5,000-10, and 000, consumption is 0.1-0.5%.
7,, it is characterized in that whole device is coupled by granulation fluidized-bed (A) and two fluidized-beds of the fluidized-bed of filming (B) to form by the used equipment of the described method of claim 1; Granulation fluidized-bed (A) is a conical fluidized bed that has pneumatic classification pipe (4), around the bedside edge, be evenly distributed with spin nozzle (13) in grid distributor (2) top, swirling eddy (10) through giving heat tangentially enters granulation fluidized-bed layer bottom by jet pipe (13), makes the bed material produce swirling motion; Grid distributor (2) is air chamber (3) and the coaxial one that is connected into of the fluidized-bed of filming (B) down; Affixed and the opening in pneumatic classification pipe (4) upper end is in grid distributor (2) central authorities, and the bottom is stretched in the fluidized-bed of filming (B), and enzyme liquid jet pipe (12) is installed in granulation fluidized-bed top; The fluidized-bed (B) of filming also is one to have the conical bed of multihole distributor; Liquefied gas (7) enters from grid distributor (6) below, and coating liquid nozzle (8) is placed in classification pipe (4) lower end, and the back product of filming is discharged from discharge gate (5); The fluidized-bed (B) of filming can not combined with granulation fluidized-bed (A) yet, but is split up into two independently fluidized-beds, cuts down with L between the two or star is cut down and linked; The granzyme product that makes from granulation fluidized-bed (A), cut down or star is cut down and directly joined in the fluidized-bed of filming (B) by L, coating liquid is from nozzle (8) the spirt bed that is installed in a top, liquefied gas (4) then enters the bed through grid distributor (6) from the bed bottom, and the membrane granule that is coated with after filming is discharged from discharge gate (5).
8, by the described equipment of claim 7, length-to-diameter ratio L/D＞15 of the pneumatic classification pipe (7) that is disposed on the fluidized-bed (A) that it is characterized in that granulating can be that straight tube also can be a lobster back.
9, by claim 7,8 described equipment, its feature is that also A bed and B bed are that one time stage pipe bottom can be equipped with one and be helped coating structure R-S, this helps coating structure system to be made up of a cone-shaped block (R) and taper reducing (S), the nozzle (8) of filming be placed on (R) and (S) between, this structure also can be applicable in the fluidized-bed (B) of filming when the A bed separates with the B bed.
10, by claim 7,9 described equipment, its feature is that also classification pipe bottom has uniform hole or groove around helping the top that is coated with structure, (Q) wrap up with wire netting (40 or 60 order) its outside, but the port area of hole groove is greater than 1.5-2.0 times of the basal area of classification pipe, and the classification air-flow enters in the classification pipe thus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90106855 CN1025156C (en) | 1990-08-22 | 1990-08-22 | Enzyme liq. fluidized bed granulation technology and apparatus thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90106855 CN1025156C (en) | 1990-08-22 | 1990-08-22 | Enzyme liq. fluidized bed granulation technology and apparatus thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1051197A CN1051197A (en) | 1991-05-08 |
| CN1025156C true CN1025156C (en) | 1994-06-29 |
Family
ID=4880303
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90106855 Expired - Fee Related CN1025156C (en) | 1990-08-22 | 1990-08-22 | Enzyme liq. fluidized bed granulation technology and apparatus thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1025156C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA02010757A (en) * | 2000-05-04 | 2004-05-17 | Dsm Nv | Process for the production of enzyme granules. |
| CN104609941B (en) * | 2014-12-23 | 2018-10-23 | 扬州雷鸥电业有限公司 | A kind of continuous sedimentation type prepares the coating drying unit and method of coated fertilizer |
| CN107115823B (en) * | 2017-06-22 | 2023-12-12 | 济川(上海)医学科技有限公司 | One-step granulator |
| CN107297295B (en) * | 2017-07-26 | 2019-10-08 | 山东禹王生态食业有限公司 | A kind of soybean protein spraying equipment and soybean protein spraying method |
| CN109368811A (en) * | 2018-11-19 | 2019-02-22 | 北京正和恒基滨水生态环境治理股份有限公司 | Microbial compound enzyme filler and preparation method thereof and application method |
-
1990
- 1990-08-22 CN CN 90106855 patent/CN1025156C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1051197A (en) | 1991-05-08 |
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