CN103341339A - High thermal stability sucralose and preparation method thereof - Google Patents
High thermal stability sucralose and preparation method thereof Download PDFInfo
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- CN103341339A CN103341339A CN2013102870423A CN201310287042A CN103341339A CN 103341339 A CN103341339 A CN 103341339A CN 2013102870423 A CN2013102870423 A CN 2013102870423A CN 201310287042 A CN201310287042 A CN 201310287042A CN 103341339 A CN103341339 A CN 103341339A
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Abstract
The invention discloses high thermal stability sucralose and a preparation method thereof. The high thermal stability sucralose is granulated. The preparation method comprises the following steps of: adding smashed crystal sucralose micro-powder, the granule diameter D97 of which is less than 30 microns, into granulation equipment, carrying out high-velocity mixing on the crystal sucralose micro-powder, and meanwhile, spraying water or a sucralose water solution with the concentration of 10%-50% (w/w%) through a pressure spraying system to obtain a binder; controlling the temperature at the range of 20-60 DEG C in a granulation process, and meanwhile, opening a cutting blade to cut a block mass after sucralose bonding, thus forming granules with loose porous microstructures and the granule diameter ranging from 50 to 800 microns; and drying the granules in a dryer so as to obtain a material the moisture content of which is 0.05%-0.2%, shaping the material in a granule shaping unit, and screening the material subjected to granule shaping through a screening machine, wherein the granule diameter is controlled through replacing meshes with different hole diameters. The screened granules are white and almost spherical, are good in mobility, and have repose angles of 25-40 degrees.
Description
Technical field
The present invention relates to product of a kind of Sucralose with high thermal stability and preparation method thereof, belong to the technical field of Sucralose preparation.Compare with the crystalloid Sucralose, product of the present invention at high temperature has the heat endurance of improvement.
Background technology
Sucralose (Sucralose) be unique be the functional sweetener of raw material with sucrose, sugariness can reach 600 times of sucrose.This sweetener has noenergy, the sugariness height, and sweet taste is pure, and characteristics such as high safety, stable in properties are one of present classic functional sweeteners.Through long-term toxicity, pharmacological evidence its tight security.Just because of the so many excellent specific property of Sucralose, it has obtained using widely in food and medicine trade.
Sucralose has formed mixed system at neutralize other composition of food, and because its concentration is lower, stability better in food system.But dry pure product Sucralose crystal heat endurance is relatively poor.
Heat endurance refers to molecule stability at high temperature, and different materials has different heat endurances, and the ability of more stable molecule antagonism thermal decomposition is more strong.Thermal decomposition then refers to material chemical cracking at high temperature.Thermal decomposition process is that at first the molecule heat absorption reaches the activation energy break chemical bonds, and atom or group reconfigure and generate pyrolysis product and release heat then.Differential thermal studies show that for organic substances such as Sucraloses, because absorbing heat greater than heat release, its DSC spectrogram demonstrates an endothermic peak usually.
Sucralose is a kind of white crystalline powder, be considered to have 130 ℃ of fusing points traditionally, yet nearest differential thermal analysis result shows Sucralose and namely observes decomposition at 119 ℃, discharge two molecular waters and a part hydrogen chloride (G.Bannach, Ecl é tica Qu í mica, 34 (9), 21-26,2009).Show that in scientific research, production and use Sucralose process, people also have new knowledge to its character constantly.In addition, MSDS(Material Safety Data Sheet according to Sucralose), requirement is avoided it is placed (＞38 ℃ of hot environments for a long time in production, storage and transportation, or＞100 ℉), even this just means that the high-purity Sucralose is under the temperature far below 119 ℃, decomposition inconspicuous (must could detect by naked eyes or instrument through the certain hour accumulation) also might take place slowly to reach.Have to studies show that under 35 ℃ condition, the phenomenon of flavescence is just arranged through 12 all trichlorine sucrose crystals; At 90 ℃-100 ℃, only need several minutes pure product Sucraloses that more great decomposition will take place, effective content reduces.
Find in the practice that the heat endurance of chemical substance is not only relevant with chemical property, also relevant with physical property.For solid particle, the physical property relevant with heat endurance comprises: granule-morphology, particle diameter, particle diameter distribution, surface roughness, bulk density and heap volume etc.At present in bibliographical information, the researcher still has different results of study and different explanations for practical physical character to the influence of heat endurance, sometimes in addition knot synthetic fibre that can be contradictory (such as distributing for particle diameter, some researchs think that the particle diameter more narrow then heat endurance that distributes is more strong; And other researchs are thought under the identical average grain diameter, and particle diameter distributes more wide, and the particle contact area increases during accumulation, be conducive to heat radiation, therefore heat endurance increases on the contrary), but the physical property of generally generally acknowledging particle determines its pyroconductivity, and the latter has crucial effects to heat endurance.In general the heat conduction is more fast, and then the heat of thermal decomposition generation can be got in time and disperse away, has avoided pyrolysis further to take place.
Tate﹠amp; Lyle company has announced a kind of technology of fluidized bed coating production particle Sucralose in the US Patent No. 7750146 of its application, obtaining certain effect aspect product flowability, anti-dust and the anti-caking, but the particle Sucralose heat endurance of this explained hereafter is improved at all, under 70 ℃ of conditions through 14.5 hours, great degraded, brown stain fully take place in product, and effective content reduces more than 50%.And the fluidized bed coating granulating process requires harsh for equipment, the control parameter is more, and it is higher that technology is amplified difficulty, is unfavorable for large-scale production.
China is the big producing country of Sucralose, and the main consumption market of Sucralose then is American-European countries.In foreign trade circulation, Sucralose must stand different temperature environments.Some unavoidable hot environments as the sunlight direct projection in the sea-freight, will influence purity and the quality of Sucralose product.And the provision for thermal insulation in increase storage and the transportation, the cost of also will increasing export greatly.Therefore for the Sucralose product, the heat endurance under its high temperature by changing its physical arrangement, improves aborning in enterprise, has very important significance.
Summary of the invention
Technical problem: the present invention is directed to the thermally-stabilised present situation of product and the deficiency of existing granulating process, explore a kind of high thermal stability Sucralose product and granulating process thereof, this process control parameter is less, and the heat endurance of product has obtained improvement, is fit to technology and amplifies.
Technical scheme: the preparation method of a kind of high thermal stability Sucralose of the present invention is: 1. the preparation method of a high thermal stability Sucralose, it is characterized in that this preparation method is: the particle diameter D97(particle diameter after will pulverizing accounts for 97% less than the particle of this numerical value, be commonly used to represent the size indicator of powder butt end) join in the Granulation Equipments less than the crystallization Sucralose micro mist of 30um, when rotating speed is not less than the 2500rpm high-speed stirred, by the gunite system spray into water or concentration be the 10%-50%w/w% aqueous solution of sucrose trichloride as binding agent, the adding mode of binding agent is evenly to spray into by the whitewashing system in the process of material dynamic motion; Carry out granulation then, the granulation process temperature is controlled in 20 ℃ of-60 ℃ of scopes, opens cutting blade simultaneously, finishes the cutting to Sucralose bonding back agglomerate, forms particle diameter has loose shape porous crack microstructure between 50um-800um granule; Again this granule is put into and obtained moisture after the drier drying and behind the material of 0.05%-0.2%w/w%, in the particle shaping unit, carry out whole grain again, realize control to grain diameter by the net sheet of changing different apertures, at last with the material behind the whole grain through the screening machine screening; Sucralose particle appearance after the screening is the nearly spherical particle of white, compares good fluidity with original crystallization Sucralose, has the angle of repose between 25 °-40 °; Particle size distribution range is narrow, and granule strength is bigger, is not easy because of the broken undesirable dust of commercial Application that produces.
Described adhesive is water or the aqueous solution of sucrose trichloride of concentration in 10%-50%w/w% scope, and wherein the weight ratio of binding agent and Sucralose micro mist is between 1:15-1:5.
The microstructure of this high thermal stability Sucralose particle is compared its inside with original crystallization Sucralose have many hole shape structures, have the loose bulk density between 0.4g/L-0.8g/L, and form oarse-grained initial superfines particle diameter D97 less than 30um.
Beneficial effect: the Sucralose by manufacturing of the present invention is graininess, can not produce dust in application process; Compare with the crystallization Sucralose of same particle sizes after screening is chosen, its consoluet time is about the former 1/3; In transportation and storage process, do not need painstakingly to control temperature, can be not the same with the crystalloid Sucralose, the jaundice owing to temperature control is not good at causing has high relatively heat endurance.
Sucralose particle among the present invention can have subsphaeroidal grain shape, good fluidity, antistatic, almost do not have a dust.Described prilling process is to add the Sucralose micro mist in the wet-mixing Granulation Equipments, in operations such as the adhesive that rotates the process adding proper proportion of mixing are at a high speed cut simultaneously, again by namely forming the Sucralose particle behind the fluidized bed drying.The Sucralose particle that this inventive method is produced, under 70 degrees centigrade condition 14.5 hours outward appearances of baking almost no change and effective content still can reach more than 90%, this is the not available characteristic of particle Sucralose of original crystalline product and other explained hereafter.
Description of drawings
Fig. 1 is the microstructure after the high thermal stability Sucralose amplifies 25 times,
Fig. 2 is the microstructure after the high thermal stability Sucralose amplifies 300 times,
Fig. 3 is the microstructure after the high thermal stability Sucralose amplifies 5000 times.
The specific embodiment
The present invention realizes by following techniqueflow:
Be added to after the original crystallization of dried Sucralose fully pulverized and mix in the granulator, under the condition that high-speed stirred is disperseed, equably pre-configured adhesive is sprayed in the comminutor by the whitewashing system, under the high-speed cutting condition of granulation blade, mixed moistening material is cut into molecule; Use the particle profile to regulate unit under material moisture state or dried condition material particles is handled, it is good that the particle Sucralose after the processing can have subsphaeroidal outward appearance and good flowability and anti-caking performance and antistatic behaviour.
The Sucralose micro mist is characterized in that after the pulverizing described in the present invention, and D97 is less than 30um.The grinding mode of realizing this fineness can be that the mechanical shock pulverizing also can be that air-flow is pulverized.
Described binding agent is technology with purified water or concentration at 10%-50%(w/w%) between sucralose solution.
The adhesive temperature that is used for the whitewashing system should be controlled between 40 ℃-60 ℃, and the endocorpuscular molding effect of this temperature range is better.
Adhesive should evenly be sent the powder in comminutor forth in 10 minutes-12 minutes, realize evenly mixing.
The weight ratio of binding agent and sucralose powder is preferably 1:10 between 1:15-1:5
Following example is only for setting forth the present invention; protection scope of the present invention is not limited to following embodiment; described those skilled in the art need figure out; this technology belongs to the granulation of powder lamination method in essence; other powder lamination method prilling all can take a hint from content of the present invention and parameter, reaches the purpose of improving Sucralose particle heat endurance.
Embodiment 1
Add the 80kg sucralose powder in the granulation unit, particle size range is D97＜30um, and the rotating speed of control comminutor paddle is 150rpm, and the rotating speed of cutting knife is 2500rpm, and powder was disperseed three minutes.Be 45 ℃ with temperature by the whitewashing system in 10 minutes then, weight is that the water of 8kg joins in the comminutor, and the rotating speed with cutting knife rises to 2800rpm simultaneously, cuts granulation.After granulation is finished the moist wood that forms transferred to and carry out drying in the fluid bed, be about 2 hours drying time.Dried material is by the particle shaping unit, and the net sheet that adds suitable aperture as requested carries out particle shaping, and the particle after the shaping through the screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 2
In the granulation unit, add the 80kg sucralose powder, its D97＜25um, the rotating speed of control paddle is 120rpm, the rotating speed of cutting knife is 2500rpm, and powder was disperseed three minutes.Be 55 ℃ with temperature by the whitewashing system in 10 minutes then, weight is that 25% sucralose solution of 9kg joins in the comminutor, and the rotating speed with cutting knife rises to 2800rpm simultaneously, cuts granulation.After granulation is finished the moist wood that forms transferred to and carry out drying in the fluid bed, be about 2 hours drying time.The dried material of dried granular material is by the particle shaping unit, and the net sheet that adds suitable aperture as requested carries out particle shaping, and the particle after the shaping through the screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 3
In the granulation unit, add the 80kg sucralose powder, its D97＜20um, the rotating speed of control paddle is 100rpm, the rotating speed of cutting knife is 2200rpm, and powder was disperseed three minutes.Be 60 ℃ with temperature by the whitewashing system in 10 minutes then, weight is that 30% sucralose solution of 9kg joins in the comminutor, and the rotating speed with cutting knife rises to 2800rpm simultaneously, cuts granulation.After granulation is finished the moist wood that forms transferred to and carry out drying in the fluid bed, be about 2 hours drying time.Dried material sieves according to particle requirement earlier, remaining bulky grain and agglomerate are by the particle shaping unit, the net sheet that adds suitable aperture as requested carries out particle shaping, and the particle after the shaping through the screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 4
With embodiment 1-3 form product that product and fluidized bed coating form, original crystalline product after sieving (require granularity close), place 70 ℃ baking oven jointly, 14.5 carry out the heat endurance evaluation after individual hour: the particle Sucralose effective content of explained hereafter of the present invention still keeps more than 90%, and the intensity with preferable heat endurance and particle is good.
Claims (3)
1. the preparation method of a high thermal stability Sucralose, it is characterized in that this preparation method is: the particle diameter D97 after will pulverizing joins in the Granulation Equipments less than the crystallization Sucralose micro mist of 30um, when rotating speed is not less than the 2500rpm high-speed stirred, by the gunite system spray into water or concentration be the 10%-50%w/w% aqueous solution of sucrose trichloride as binding agent, the adding mode of binding agent is evenly to spray into by the whitewashing system in the process of material dynamic motion; Carry out granulation then, the granulation process temperature is controlled in 20 ℃ of-60 ℃ of scopes, opens cutting blade simultaneously, finishes the cutting to Sucralose bonding back agglomerate, forms particle diameter has loose shape porous crack microstructure between 50um-800um granule; Again this granule is put into and obtained moisture after the drier drying and behind the material of 0.05%-0.2%w/w%, in the particle shaping unit, carry out whole grain again, realize control to grain diameter by the net sheet of changing different apertures, at last with the material behind the whole grain through the screening machine screening; Sucralose particle appearance after the screening is the nearly spherical particle of white, compares good fluidity with original crystallization Sucralose, has the angle of repose between 25 °-40 °; Particle size distribution range is narrow, and granule strength is bigger, is not easy because of the broken undesirable dust of commercial Application that produces.
2. the preparation method of high thermal stability Sucralose as claimed in claim 1, it is characterized in that described adhesive is water or the aqueous solution of sucrose trichloride of concentration in 10%-50%w/w% scope, wherein the weight ratio of binding agent and Sucralose micro mist is between 1:15-1:5.
3. the high thermal stability Sucralose of a preparation method as claimed in claim 1 preparation, the microstructure that it is characterized in that this high thermal stability Sucralose particle is compared its inside with original crystallization Sucralose have many hole shape structures, have the loose bulk density between 0.4g/L-0.8g/L, and form oarse-grained initial superfines particle diameter D97 less than 30um.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104026549A (en) * | 2014-05-30 | 2014-09-10 | 翁源广业清怡食品科技有限公司 | Preparation method of granular sucralose |
| CN108058283A (en) * | 2017-12-14 | 2018-05-22 | 烟台只楚化学新材料股份有限公司 | A kind of polyolefin transparent nucleater particle and preparation method thereof of high-purity, high fluidity |
| CN112806551A (en) * | 2020-12-30 | 2021-05-18 | 翁源广业清怡食品科技有限公司 | Granulation production method for improving thermal stability of sucralose |
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| CN1449253A (en) * | 2000-08-04 | 2003-10-15 | 阿迪索法国两合公司 | Process for the preparation of granules of methionine |
| US20050203290A1 (en) * | 2003-04-30 | 2005-09-15 | Catani Steven J. | Crystalline form of sucralose, and method for producing it |
| CN101184404A (en) * | 2005-03-18 | 2008-05-21 | 塔特和莱利技术有限公司 | Granular sucralose, and method of making it |
| CN102977157A (en) * | 2012-12-05 | 2013-03-20 | 溧阳维信生物科技有限公司 | Crystallization method for sucralose |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449253A (en) * | 2000-08-04 | 2003-10-15 | 阿迪索法国两合公司 | Process for the preparation of granules of methionine |
| US20050203290A1 (en) * | 2003-04-30 | 2005-09-15 | Catani Steven J. | Crystalline form of sucralose, and method for producing it |
| CN101184404A (en) * | 2005-03-18 | 2008-05-21 | 塔特和莱利技术有限公司 | Granular sucralose, and method of making it |
| CN102977157A (en) * | 2012-12-05 | 2013-03-20 | 溧阳维信生物科技有限公司 | Crystallization method for sucralose |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104026549A (en) * | 2014-05-30 | 2014-09-10 | 翁源广业清怡食品科技有限公司 | Preparation method of granular sucralose |
| CN108058283A (en) * | 2017-12-14 | 2018-05-22 | 烟台只楚化学新材料股份有限公司 | A kind of polyolefin transparent nucleater particle and preparation method thereof of high-purity, high fluidity |
| CN112806551A (en) * | 2020-12-30 | 2021-05-18 | 翁源广业清怡食品科技有限公司 | Granulation production method for improving thermal stability of sucralose |
| CN112806551B (en) * | 2020-12-30 | 2023-09-15 | 翁源广业清怡食品科技有限公司 | Granulating production method for improving heat stability of sucralose |
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