CN101486741A - Process for continuous production of crystal maltose alcohol - Google Patents

Process for continuous production of crystal maltose alcohol Download PDF

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Publication number
CN101486741A
CN101486741A CNA200810238346XA CN200810238346A CN101486741A CN 101486741 A CN101486741 A CN 101486741A CN A200810238346X A CNA200810238346X A CN A200810238346XA CN 200810238346 A CN200810238346 A CN 200810238346A CN 101486741 A CN101486741 A CN 101486741A
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temperature
crystal
discharging
maltitol
cooling
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CN101486741B (en
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熊先锋
李令平
孙鲁
赵光辉
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Qingdao honey good fortune hall health Science and Technology Ltd.
Shandong Futaste Co.,Ltd.
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Shandong Futian Investment Co Ltd
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Abstract

The invention relates to a process for successively producing crystal maltol, which can realize large-sized material crystallization, resolves the problem that crystallization can not be successive during the production of crystal maltol and realizes the successive in and out of material and the successive operation of production. Above all, the multilayer coiled pipe ladder hypothermy leads the material to be even and controllable and have good crystallization efficiency. In addition, the process can also reduce the labor intensity of workers.

Description

A kind of technology of continuous production crystal maltitol
Technical field
The present invention relates to a kind of technology of continuous production crystal maltitol, especially a kind of processing method of utilizing vertical continuous crystallisation jar continuous production crystal maltitol belongs to technical field of functional sugar alcohol production.
Background technology
Maltose alcohol is a kind of functional sweetener, is generally prepared through hydrogenation by maltose.Because of it has high sugariness, high stability, is difficult for causing characteristics such as fermentation using bacteria, be widely used in low food and the diabetic subject's food in low heat value, fat-reducing with to teeth corrosion.Because maltose alcohol is easy to moisture absorption, easy deliquescence, thereby is difficult to crystallization, and the transportation of liquid maltose alcohol is inconvenient with use.For addressing this problem, a lot of technical schemes with the maltose alcohol crystallization have been proposed.But no matter be domestic at present or be to utilize horizontal crystallizer in the world mostly, adopt the intermittent type crystallization process to carry out the maltose alcohol crystallization, promptly at first horizontal crystallizer is filled with material,, add the crystal seed assisting crystallisation of some amount in the process then according to the temperature lowering curve gradient cooling, whole jar of temperature of charge is identical, by same gradient cooling, finish up to crystallisation process, after crystallization is finished, material is all delivered to separation circuit, charging again then in the crystallizer.There is various disadvantages in this production technique: the crystallizing cycle of (1) every crystallizer all comprises independent charging, adds crystal seed, growing the grain, discharging time, has caused that crystallizing cycle is long, production efficiency is low; (2) the crystallizer capacity is little, just must increase the quantity of crystallizer as enlarging output, and frequent operation can expend a large amount of man power and materials; (3) crystallizer adopts the chuck cooling, and material is heated inhomogeneous, overall cooling of influence and crystallization effect; (4) crystallizer stirring wing and crystal grain friction are easy to generate metallic impurity and make the crystal grain fragmentation.
Chinese patent 200520078682.4, the continuous cooling crystallizer of a kind of multistage coil pipe oscillatory type is disclosed, mention in the literary composition and can divide into groups to control to cooling unit according to the difference of processing parameter, the crystallisation process of material is carried out smoothly, but for different raw materials different processing methodes is arranged, do not relate in the literary composition; The patent No. is that 07/14953B discloses a kind of maltose alcohol molasses crystalline manufacture method that contains, this method offers the forcing machine with elongated cooling zone and kneading district continuously with the aqueous solution of maltose alcohol, in the presence of crystal seed, cool off continuously and integrate, obtain maltose alcohol cream, from nozzle, sugar alcohol cream is extruded continuously then, obtain containing the crystal of maltose alcohol molasses, although this method is being succeeded aspect the use operation serialization, but used forcing machine with elongated cooling zone, in order to carry out the concentration process of high density, temperature uprises inevitably, be unfavorable for later crystallisation by cooling, and the maltitol pulp of high density causes viscosity to become big because cooling descends temperature, needs powerful equipment when integrating operation, and running cost is increased; Chinese patent 200710018179.3 discloses the production technique of a kind of crystal diabetin on vertical continuous crystallizer, disclosed the applicable cases of vertical continuous crystallizer on crystal diabetin is produced, but this processing method can not be used for instructing or directly applying to the production crystal maltitol.
Summary of the invention
At the deficiency that exists on the existing crystal maltitol production technique, technical problem to be solved by this invention is, a kind of technology of continuous production crystal maltitol is provided, with the problem that maltose alcohol continuous crystallisation and material in the solution production process are back to back, realize the serialization operation of producing.
For solving described technical problem, the technical solution used in the present invention is, a kind of technology of continuous production crystal maltitol, and it comprises following content:
A, be 30-90% with maltitol pulp evaporation concentration to dry biomass percentage concentration, maltose alcohol content 〉=92% in its dry-matter, adjusting temperature is 55-85 ℃;
B, the gained material is squeezed into vertical continuous crystallisation jar, treat material arrive liquid level 5-20% the time, the hydraulic pressure that starts jar end stirs;
C, when material in the crystallizer during apart from 0.5-3.0 meters of tank decks, stop charging, start cooling system circulation pump, to the material growing the grain of lowering the temperature; In whole temperature-fall period, the difference of spiral coil cooling tube water temperature and temperature of charge is 2-8 ℃; Be provided with separately independently upper, middle and lower three cover refrigerating units in the crystallizer, reducing once the temperature of each layer water coolant in per 2 hours sets, form gradually and go up the low gradient of relative superiority or inferiority, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow be controlled at the 10-25 cubic meter/hour; The temperature difference of spiral coil cooling tube water and temperature of charge needs control, because the too big temperature difference can cause the formation of a large amount of nucleus, increases the slurry viscosity, thereby reduces separation efficiency.
D, through 50~70 hours cooling growing the grains, when crystallization yield reaches butt 40-50%, get final product discharging;
When e, discharging, open bleeder valve, start the discharging pump discharging, open the kind recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed, and opens the feed valve charging, regulates charging, discharging flow, keeps the canful operation;
F, the crystal maltitol cream of gained is centrifugal, oven dry, packing obtain maltose alcohol content and are 99.00-99.99% crystal maltitol finished product.
Optimize, the technology of above-mentioned continuous production crystal maltitol comprises following content:
A, be 76-80% with maltitol pulp evaporation concentration to dry biomass percentage concentration, maltose alcohol content 92-95% in its dry-matter, adjusting temperature is 65-75 ℃;
B, the gained material is squeezed into vertical continuous crystallisation jar, treat material arrive liquid level 8-15% the time, the hydraulic pressure that starts jar end stirs;
C, when material in the crystallizer during apart from 0.8-1.5 meters of tank decks, stop charging, start cooling system circulation pump, to the material growing the grain of lowering the temperature; In whole temperature-fall period, the difference of spiral coil cooling tube water temperature and temperature of charge is 2-8 ℃; Be provided with separately independently upper, middle and lower three cover refrigerating units in the crystallizer, reducing once the temperature of each layer water coolant in per 2 hours sets, form gradually and go up the low gradient of relative superiority or inferiority, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow be controlled at the 13-18 cubic meter/hour;
D, through 55~64 hours cooling growing the grains, when crystallization yield reaches butt 42-48%, get final product discharging;
When e, discharging, open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed, and opens the feed valve charging, regulates charging, discharging flow, keeps the canful operation;
F, the crystal maltitol cream of gained is centrifugal, the oven dry, the packing, obtain the crystal maltitol finished product.
It is 0.5-3.0 minutes reciprocating strokes that the technology of above-mentioned continuous production crystal maltitol, the described hydraulic pressure of its step b stir its frequency setting, preferred 1-2 minute reciprocating stroke.
The technology of above-mentioned continuous production crystal maltitol, the described maintenance canful operation of its step e after operation is normal, is made as the DCS reference mark automatically, by computer crystallisation process is accurately controlled.
The technology of above-mentioned continuous production crystal maltitol, the described crystal maltitol finished product of its step f, the crystal formation of its crystal maltitol has rectangular build, positive tetrahedron type and triangular pyramid type.
The present invention is applied to vertical continuous crystallizer in the maltose alcohol production, is aided with the setting of various link Parameter Optimization, thereby forms a kind of technology of continuous production crystal maltitol, can realize large-scale material crystallization.
Vertical CGS Continuous Grain Silicon of the present invention, related a kind of major equipment is a vertical continuous crystallizer, it comprises vertical continuous crystallisation jar, hydraulic efficiency system, material cooling system etc.The profile of this vertical continuous crystallizer is vertical oval tubular, and top is the plane loam cake, on cover and be provided with crossbeam, be used to install refrigerating unit and distribution device, the bottom is the conical head of compacting.Cooling system is to be made by symmetric shape spiral coil cooling tube of typing, is fixed on the fall way, can swing up and down to material and cause certain impact that material is rotated stirring.The vertical shifting of refrigerating unit is produced by the hydro-cylinder that is installed in the crystallizer top, and hydraulic efficiency plant produces the speed of two vertical shifting, and this design does not need the support of any bearing or stuffing box.
During crystallizer work, need the crystalline material to send into crystallizer from the top with pump, and by the agitator uniform distribution, material is by impacting impellent, pass through piece type spiral coil cooling tube successively, the material that crystallization finishes is discharged from the bottom, water coolant enters water-cooled tube by flexible pipe, from the overhead stream to the bottom, flow back into top and material convection current again, also played self cleanup action when coil pipe moves up and down in material, as long as spiral coil cooling tube is all the time below liquid level and keep the crystallization cooling curve, just can guarantee that crystallization is clear and coherent continuously, form the charging of material, crystallization, the running balance of discharging realizes continuous crystallisation, and production efficiency improves greatly.The operation of this system can be controlled by DCS, and the unmanned management of realize producing is enhanced productivity and the accuracy of production control greatly.
The invention has the beneficial effects as follows: (1) solves in the crystal maltitol production process crystallization can not the successive problem, realizes the continuous operation of being back to back and producing of material; (2) multilayer coil pipe step cooling makes material lowering temperature uniform, controlled, and crystallization effect is good; (3) reduce working strength of workers.
Equipment involved in the present invention is existing installation, and related material is an industry raw material commonly used, all buys on market.
Detection method involved in the present invention is the usual method of using of the industry.
Description of drawings
The present invention is further illustrated below in conjunction with drawings and the specific embodiments.
Fig. 1 is the crystal formation figure that uses the crystal maltitol of prepared of the present invention.
Embodiment
Embodiment 1:
(1) according to a conventional method with W-Gum behind α-Dian Fenmeiyehua, generate enzyme glycolysis through beta-amylase, Pullulanase and maltose again, obtain malt syrup, with this malt syrup hydrogenation, obtain maltitol solution, again through decolouring, from hand over, to obtain mass percent concentration be 76% maltitol pulp in evaporation, its maltose alcohol content is 93%, temperature is 75 ℃, and this material is squeezed in the vertical continuous crystallisation jar;
(2) treat that material arrives 10% o'clock of liquid level, the stirring and the hydraulic pressure that start jar end stir, and the frequency setting that hydraulic pressure is stirred is two minutes reciprocating strokes;
(3) when material during, stop charging, start cooling system circulation pump, the material growing the grain of lowering the temperature apart from about 1 meter of tank deck.Reduced once the temperature of each layer water coolant in per 2 hours and set, and form the upward low gradient of relative superiority or inferiority gradually, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow is controlled at 13 cubic metres/hour;
(4) through 55 hours cooling growing the grain,, promptly reach the opportunity of discharging when crystallization yield reaches 42% (butt);
(5) open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed;
(6) open the feed valve charging, regulate charging, discharging flow, keep the canful operation;
(7) crystal alcohol cream obtains maltose alcohol content and is 99.3% crystal maltitol finished product through centrifugal, oven dry, packing.
Embodiment 2:
(1) according to a conventional method with W-Gum behind α-Dian Fenmeiyehua, generate enzyme glycolysis through beta-amylase, Pullulanase and maltose again, obtain malt syrup, with this malt syrup hydrogenation, obtain maltitol solution, again through decolouring, from hand over, to obtain mass percent concentration be 80% maltitol liquor in evaporation, its maltose alcohol content is 95%, temperature is 70 ℃, and this material is squeezed in the vertical continuous crystallisation jar;
(2) treat that material arrives 15% o'clock of liquid level, the stirring and the hydraulic pressure that start jar end stir, and the frequency setting that hydraulic pressure is stirred is one minute reciprocating stroke;
(3) when material during, stop charging, start cooling system circulation pump, the material growing the grain of lowering the temperature apart from about 1.5 meters of tank deck.Reduced once the temperature of each layer water coolant in per 2 hours and set, and form the upward low gradient of relative superiority or inferiority gradually, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃.Cooling water flow is controlled at 15 cubic metres/hour;
(4) through 60 hours cooling growing the grain, when crystallization yield reaches 45% (butt), promptly reach the opportunity of discharging;
(5) open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed;
(6) open the feed valve charging, regulate charging, discharging flow, keep the canful operation;
(7) crystal alcohol cream obtains maltose alcohol content and is 99.7% crystal maltitol finished product through centrifugal, oven dry, packing.
Embodiment 3:
(1) according to a conventional method with W-Gum behind α-Dian Fenmeiyehua, generate enzyme glycolysis through beta-amylase, Pullulanase and maltose again, obtain malt syrup, with this malt syrup hydrogenation, obtain maltitol solution, again through decolouring, from hand over, to obtain mass percent concentration be 78% maltitol liquor in evaporation, its maltose alcohol content is 92%, temperature is 65 ℃, and this material is squeezed in the vertical continuous crystallisation jar;
(2) treat that material arrives 8% o'clock of liquid level, the stirring and the hydraulic pressure that start jar end stir, and the frequency setting that hydraulic pressure is stirred is 1.5 minutes reciprocating strokes;
(3) when material during, stop charging, start cooling system circulation pump, the material growing the grain of lowering the temperature apart from about 0.8 meter of tank deck.Reduced once the temperature of each layer water coolant in per 2 hours and set, and form the upward low gradient of relative superiority or inferiority gradually, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow is controlled at 18 cubic metres/hour;
(4) through 64 hours cooling growing the grain, when crystallization yield reaches 48% (butt), promptly reach the opportunity of discharging;
(5) open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed;
(6) open the feed valve charging, regulate charging, discharging flow, keep the canful operation;
(7) crystal alcohol cream obtains maltose alcohol content and is 99.6% crystal maltitol finished product through centrifugal, oven dry, packing.
Embodiment 4:
(1) according to a conventional method with W-Gum behind α-Dian Fenmeiyehua, generate enzyme glycolysis through beta-amylase, Pullulanase and maltose again, obtain malt syrup, with this malt syrup hydrogenation, obtain maltitol solution, again through decolouring, from hand over, to obtain mass percent concentration be 30% maltitol pulp in evaporation, its maltose alcohol content is 94%, temperature is 85 ℃, and this material is squeezed in the vertical continuous crystallisation jar;
(2) treat that material arrives 20% o'clock of liquid level, the stirring and the hydraulic pressure that start jar end stir, and the frequency setting that hydraulic pressure is stirred is three minutes reciprocating strokes;
(3) when material during, stop charging, start cooling system circulation pump, the material growing the grain of lowering the temperature apart from about 0.5 meter of tank deck.Reduced once the temperature of each layer water coolant in per 2 hours and set, and form the upward low gradient of relative superiority or inferiority gradually, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow is controlled at 25 cubic metres/hour;
(4) through 70 hours cooling growing the grain,, promptly reach the opportunity of discharging when crystallization yield reaches 40% (butt);
(5) open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed;
(6) open the feed valve charging, regulate charging, discharging flow, keep the canful operation; After operation is normal, the DCS reference mark is made as automatically, crystallisation process is accurately controlled by computer;
(7) crystal alcohol cream obtains maltose alcohol content and is 99.99% crystal maltitol finished product through centrifugal, oven dry, packing.
Embodiment 5:
(1) according to a conventional method with W-Gum behind α-Dian Fenmeiyehua, generate enzyme glycolysis through beta-amylase, Pullulanase and maltose again, obtain malt syrup, with this malt syrup hydrogenation, obtain maltitol solution, again through decolouring, from hand over, to obtain mass percent concentration be 90% maltitol pulp in evaporation, its maltose alcohol content is 92%, temperature is 55 ℃, and this material is squeezed in the vertical continuous crystallisation jar;
(2) treat that material arrives 5% o'clock of liquid level, the stirring and the hydraulic pressure that start jar end stir, and the frequency setting that hydraulic pressure is stirred is half a minute reciprocating stroke;
(3) when material during, stop charging, start cooling system circulation pump, the material growing the grain of lowering the temperature apart from about 3 meters of tank deck.Reduced once the temperature of each layer water coolant in per 2 hours and set, and form the upward low gradient of relative superiority or inferiority gradually, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow is controlled at 10 cubic metres/hour;
(4) through 50 hours cooling growing the grain,, promptly reach the opportunity of discharging when crystallization yield reaches 50% (butt);
(5) open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed;
(6) open the feed valve charging, regulate charging, discharging flow, keep the canful operation; After operation is normal, the DCS reference mark is made as automatically, crystallisation process is accurately controlled by computer;
(7) crystal alcohol cream obtains maltose alcohol content and is 99.0% crystal maltitol finished product through centrifugal, oven dry, packing.

Claims (6)

1, a kind of technology of continuous production crystal maltitol, it comprises following content:
A, be 30-90% with maltitol pulp evaporation concentration to dry biomass percentage concentration, maltose alcohol content 〉=92% in its dry-matter, adjusting temperature is 55-85 ℃;
B, the gained material is squeezed into vertical continuous crystallisation jar, treat material arrive liquid level 5-20% the time, the hydraulic pressure that starts jar end stirs;
C, when material in the crystallizer during apart from 0.5-3.0 meters of tank decks, stop charging, start cooling system circulation pump, to the material growing the grain of lowering the temperature; In whole temperature-fall period, the difference of spiral coil cooling tube water temperature and temperature of charge is 2-8 ℃; Be provided with separately independently upper, middle and lower three cover refrigerating units in the crystallizer, reducing once the temperature of each layer water coolant in per 2 hours sets, form gradually and go up the low gradient of relative superiority or inferiority, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow be controlled at the 10-25 cubic meter/hour;
D, through 50~70 hours cooling growing the grains, when crystallization yield reaches butt 40-50%, get final product discharging;
When e, discharging, open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed, and opens the feed valve charging, regulates charging, discharging flow, keeps the canful operation;
F, the crystal maltitol cream of gained is centrifugal, oven dry, packing obtain maltose alcohol content and are 99.00-99.99% crystal maltitol finished product.
2, technology according to claim 1, it comprises following content:
A, be 76-80% with maltitol pulp evaporation concentration to dry biomass percentage concentration, maltose alcohol content 92-95% in its dry-matter, adjusting temperature is 65-75 ℃;
B, the gained material is squeezed into vertical continuous crystallisation jar, treat material arrive liquid level 8-15% the time, the hydraulic pressure that starts jar end stirs;
C, when material in the crystallizer during apart from 0.8-1.5 meters of tank decks, stop charging, start cooling system circulation pump, to the material growing the grain of lowering the temperature; In whole temperature-fall period, the difference of spiral coil cooling tube water temperature and temperature of charge is 2-8 ℃; Be provided with separately independently upper, middle and lower three cover refrigerating units in the crystallizer, reducing once the temperature of each layer water coolant in per 2 hours sets, form gradually and go up the low gradient of relative superiority or inferiority, at last the temperature of upper, middle and lower three jacket waters is set at respectively: 35 ℃, 30 ℃, 25 ℃, cooling water flow be controlled at the 13-18 cubic meter/hour;
D, through 55~64 hours cooling growing the grains, when crystallization yield reaches butt 42-48%, get final product discharging;
When e, discharging, open bleeder valve, start the discharging pump discharging, open the crystal seed recycle pump simultaneously, the backflow partial material comes back in the vertical continuous crystallisation jar as crystal seed, and opens the feed valve charging, regulates charging, discharging flow, keeps the canful operation;
F, the crystal maltitol cream of gained is centrifugal, the oven dry, the packing, obtain the crystal maltitol finished product.
3, technology according to claim 1 and 2 is characterized in that: it is 0.5-3.0 minutes reciprocating strokes that the described hydraulic pressure of its step b stirs its frequency setting.
4, technology according to claim 3 is characterized in that: it is 1-2 minute reciprocating stroke that the described hydraulic pressure of step b stirs its frequency setting.
5, technology according to claim 4 is characterized in that: the described maintenance canful operation of its step e, it is made as the DCS reference mark automatically for after moving normally, crystallisation process is accurately controlled the canful operation by computer.
6, technology according to claim 5 is characterized in that: the described crystal maltitol finished product of its step f, the crystal formation of its crystal maltitol has rectangular build, positive tetrahedron type and triangular pyramid type.
CN200810238346XA 2008-12-15 2008-12-15 Process for continuous production of crystal maltose alcohol Active CN101486741B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101850189A (en) * 2010-03-30 2010-10-06 山东福田药业有限公司 New process for continuous crystallization of sugar alcohol and vertical continuous crystallizer
CN110938714A (en) * 2019-12-03 2020-03-31 山东福田药业有限公司 Production method of high-purity crystal maltose

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3602903B2 (en) * 1995-05-02 2004-12-15 東和化成工業株式会社 Crystal maltitol and method for producing nectar-containing crystals containing the same
US20050220959A1 (en) * 2002-06-19 2005-10-06 Ryuzo Ueno Process for producing crystalline maltitol
AU2004263221B2 (en) * 2003-07-18 2008-06-26 Cargill Incorporated Process for preparing maltitol enriched products
CN2774609Y (en) * 2005-04-27 2006-04-26 西安航天华威压力容器设备制造有限公司 Multiple stage coil pipe vibration type continuous cooling crystallizer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101850189A (en) * 2010-03-30 2010-10-06 山东福田药业有限公司 New process for continuous crystallization of sugar alcohol and vertical continuous crystallizer
CN110938714A (en) * 2019-12-03 2020-03-31 山东福田药业有限公司 Production method of high-purity crystal maltose
CN110938714B (en) * 2019-12-03 2023-08-15 山东福田药业有限公司 Production method of high-purity crystalline maltose

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