CN103341339B - A kind of High thermal stability sucralose and preparation method thereof - Google Patents
A kind of High thermal stability sucralose and preparation method thereof Download PDFInfo
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Abstract
The present invention is a kind of High thermal stability sucralose and preparation method thereof, this High thermal stability sucralose is graininess, the crystallization Sucralose micro mist that particle diameter D97 after pulverizing is less than 30um joins in Granulation Equipments by preparation method, while high-speed stirred, water is sprayed into or concentration is 10%-50%(w/w% by gunite system) aqueous solution of sucrose trichloride is as binding agent, granulation process temperature controls within the scope of 20 DEG C-60 DEG C, open cutting blade simultaneously, complete the cutting to agglomerate after Sucralose bonding, form the granule that particle diameter has loose shape concrete dynamic modulus microstructure between 50um-800um, obtain moisture after again this granule being put into drier drying and in particle shaping unit, carry out whole grain again after the material of 0.05%-0.2%, realize the control to grain diameter by the mesh sheet changing different pore size, the material after whole grain sieves through screening machine, particle appearance after screening is the nearly spherical particle of white, and good fluidity, has the angle of repose between 25 °-40 °.
Description
Technical field
The present invention relates to and a kind of there is product of the Sucralose of high thermal stability and preparation method thereof, belong to technical field prepared by Sucralose.Compare with crystalloid Sucralose, product of the present invention at high temperature has the heat endurance of improvement.
Background technology
The functional sweetener of Sucralose (Sucralose) to be unique with sucrose be raw material, sugariness can reach sucrose 600 times.This sweetener has noenergy, and sugariness is high, and sweet taste is pure, the feature such as high safety, stable in properties, is one of current classic functional sweetener.Its tight security is demonstrated through long-term toxicity, pharmacological test.Just because of the excellent specific property that Sucralose is so many, it is widely used in food and medicine trade.
Sucralose in food and other composition define mixed system, and due to its concentration lower, in food system, stability is better.But the sterling Sucralose crystal heat endurance of drying is 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 stronger.Thermal decomposition then refers to material chemical cracking at high temperature.Thermal decomposition process is that first molecule heat absorption reaches activation energy break chemical bonds, and then atom or group reconfigure and generate pyrolysis product and release heat.Differential thermal research shows, for organic substances such as Sucraloses, because heat absorption is 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 DEG C of fusing points traditionally, but namely nearest differential thermal analysis result display Sucralose observes decomposition at 119 DEG C, discharge two molecular waters and a part hydrogen chloride (G.Bannach, Ecl é ticaQu í mica, 34 (9), 21-26,2009).Show that people are also constantly having new knowledge to its character in scientific research, production and use Sucralose process.In addition, according to the MSDS (MaterialSafetyDataSheet) of Sucralose, require in production, store and avoid it being placed in for a long time hot environment (> 38 DEG C in transportation, or > 100 ℉), even if this just means that high-purity Sucralose is at the temperature far below 119 DEG C, also likely there is decomposition slow and inconspicuous (have to pass through certain hour accumulation, just detect by naked eyes or instrument).Under having research to be presented at the condition of 35 DEG C, just there is the phenomenon of flavescence through 12 weeks trichlorine sucrose crystals; At 90 DEG C-100 DEG C, only need several minutes sterling Sucraloses that more great decomposition will occur, effective content reduces.
Find in practice, 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 to heat endurance comprises: granule-morphology, particle diameter, domain size distribution, surface roughness, bulk density and heap volume etc.At present in bibliographical information, researcher still has different results of study and different explanations for Particle physical properties to the impact of heat endurance, sometimes (such as domain size distribution, some researchs think that the narrower then heat endurance of domain size distribution is stronger to knot synthetic fibre that even can be contradictory; And other researchs think that under identical average grain diameter, domain size distribution is wider, during accumulation, particle contacts area increases, be conducive to heat radiation, therefore heat endurance increases on the contrary), but generally generally acknowledge that the physical property of particle determines its pyroconductivity, and the latter has vital effect to heat endurance.In general heat transfer is faster, then the heat that thermal decomposition produces can disperse away more in time, avoids pyrolysis and occurs further.
Tate & lyle company discloses the technique that a kind of fluidized bed coating produces particle Sucralose in its US Patent No. 7750146 of applying for, certain effect is achieved in product mobility, anti-dust and anti-caking, but the particle Sucralose heat endurance of this explained hereafter is not fundamentally improved, through 14.5 hours under 70 DEG C of conditions, there is great degraded, brown stain completely in product, effective content reduces by more than 50%.And fluidized bed coating granulating process is harsh for equipment requirement, and controling parameters is more, technique amplification difficulty is higher, is unfavorable for large-scale production.
China is the big producing country of Sucralose, and the major consumers market Ze Shi American-European countries of Sucralose.In foreign trade circulation, Sucralose must stand different temperature environments.Some unavoidable hot environments, as the direct sunlight in sea-freight, will affect purity and the quality of Sucralose product.And increase the provision for thermal insulation stored and in transport, cost of also greatly increasing export.Therefore for Sucralose product, enterprise by changing its physical arrangement, improving the heat endurance under its high temperature, having very important significance aborning.
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 obtains improvement, is applicable to technique and amplifies.
Technical scheme: the preparation method of a kind of High thermal stability sucralose of the present invention is: the 1. preparation method of a High thermal stability sucralose, it is characterized in that this preparation method is: (particle that particle diameter is less than this numerical value accounts for 97% by the particle diameter D97 after pulverizing, being commonly used to the size indicator representing powder butt end) the crystallization Sucralose micro mist that is less than 30um joins in Granulation Equipments, while rotating speed is not less than 2500rpm high-speed stirred, water is sprayed into or concentration is that 10%-50%w/w% aqueous solution of sucrose trichloride is as binding agent by gunite system, the feed postition of binding agent is evenly sprayed into by spraying system in the process of material dynamic motion, then carry out granulation, granulation process temperature controls, within the scope of 20 DEG C-60 DEG C, to open cutting blade simultaneously, completes the cutting to agglomerate after Sucralose bonding, forms the granule that particle diameter has loose shape concrete dynamic modulus microstructure between 50um-800um, obtain moisture after again this granule being put into drier drying and in particle shaping unit, carry out whole grain again after the material of 0.05%-0.2%w/w%, realize the control to grain diameter by the mesh sheet changing different pore size, finally the material after whole grain is sieved through screening machine, Sucralose particle appearance after screening is the nearly spherical particle of white, and good fluidity compared with initial crystalline Sucralose, has the angle of repose between 25 °-40 °, particle size distribution range is narrow, and granule strength is comparatively large, is not easy to produce the undesirable dust of commercial Application because of broken.
Described adhesive is water or the aqueous solution of sucrose trichloride of concentration within the scope of 10%-50%w/w%, and wherein the weight ratio of binding agent and Sucralose micro mist is between 1:15-1:5.
There are many hole shape structures microstructure its inside compared with initial crystalline Sucralose of this High thermal stability sucralose particle, there is the loose bulk density between 0.4g/mL-0.8g/mL, and form oarse-grained initial superfines particle diameter D97 and be less than 30um.
Beneficial effect: the Sucralose manufactured by the present invention is graininess, can not produce dust in application process; Compared with the crystallization Sucralose of the same particle sizes after choosing with screening, its consoluet time is about the former 1/3; Deliberately control temperature is not needed in transport and storage process, can not be the same with crystalloid Sucralose, the jaundice caused because temperature controls to be not good at, has relatively high heat endurance.
Sucralose particle in the present invention can have subsphaeroidal grain shape, good fluidity, antistatic, almost without dust.Described prilling process for add Sucralose micro mist in wet-mixing Granulation Equipments, and the adhesive adding proper proportion in the process of High Rotation Speed mixing such as to be cut at the operation simultaneously, more namely forms Sucralose particle by after fluidized bed drying.The Sucralose particle that this inventive method is produced, under the condition of 70 degrees Celsius, toast that 14.5 hours outward appearances are almost unchanged and effective content still can reach more than 90%, this is the characteristic not available for particle Sucralose of initial crystalline product and other explained hereafter.
Accompanying drawing explanation
Fig. 1 is the microstructure that High thermal stability sucralose amplifies after 25 times,
Fig. 2 is the microstructure that High thermal stability sucralose amplifies after 300 times,
Fig. 3 is the microstructure that High thermal stability sucralose amplifies after 5000 times.
Detailed description of the invention
The present invention is realized by following techniqueflow:
Being added to after fully being pulverized by dried Sucralose initial crystalline is uniformly mixed in granulator, equably pre-configured adhesive is sprayed in comminutor by spraying system under the condition of high-speed stirred dispersion, under the high-speed cutting condition of granulation blade, mixed moistening material is cut into molecule; Under material moisture state or dried condition, use particle profile to regulate unit to process material particles, the particle Sucralose after process can have subsphaeroidal outward appearance and good mobility and anti-caking performance and antistatic behaviour good.
After pulverizing described in the present invention, Sucralose micro mist, is characterized in that, D97 is less than 30um.The grinding mode realizing this fineness can be that mechanical shock pulverizes also can be air-flow crushing.
Described binding agent is technique purified water or the sucralose solution of concentration between 10%-50% (w/w%).
Adhesive temperature for spraying system should control between 40 DEG C-60 DEG C, and the endocorpuscular molding effect of this temperature range is better.
Adhesive should evenly send the powder in comminutor forth in 10 minutes-12 minutes, realized Homogeneous phase mixing.
The weight ratio of binding agent and sucralose powder, between 1:15-1:5, is preferably 1:10
Following instance is only elaboration the present invention; protection scope of the present invention is not limited to following embodiment; described those skilled in the art need understand; this technique belongs to the granulation of powder bed area method in essence; other powder bed area method prilling all can take a hint from content of the present invention and parameter, reaches the object improving Sucralose particle heat endurance.
Embodiment 1
In granulation unit, add 80kg sucralose powder, particle size range was D97<30um, and the rotating speed controlling comminutor paddle is 150rpm, and the rotating speed of cutting knife is 2500rpm, by powder dispersion three minutes.Then be 45 DEG C by temperature by spraying system in 10 minutes, weight is that the water of 8kg joins in comminutor, the rotating speed of cutting knife is risen to 2800rpm simultaneously, carries out cutting granulation.After granulation completes, the moist wood of formation is transferred in fluid bed and carry out drying, be about 2 hours drying time.Dried material is by particle shaping unit, and the mesh sheet of adding suitable aperture as requested carries out particle shaping, and the particle after shaping through screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 2
In granulation unit, add 80kg sucralose powder, its D97<25um, controlling the rotating speed of paddle was 120rpm, and the rotating speed of cutting knife is 2500rpm, by powder dispersion three minutes.Then be 55 DEG C by temperature by spraying system in 10 minutes, weight is that 25% sucralose solution of 9kg joins in comminutor, the rotating speed of cutting knife is risen to 2800rpm simultaneously, carries out cutting granulation.After granulation completes, the moist wood of formation is transferred in fluid bed and carry out drying, be about 2 hours drying time.The dried material of dried granular material is by particle shaping unit, and the mesh sheet of adding suitable aperture as requested carries out particle shaping, and the particle after shaping through screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 3
In granulation unit, add 80kg sucralose powder, its D97<20um, controlling the rotating speed of paddle was 100rpm, and the rotating speed of cutting knife is 2200rpm, by powder dispersion three minutes.Then be 60 DEG C by temperature by spraying system in 10 minutes, weight is that 30% sucralose solution of 9kg joins in comminutor, the rotating speed of cutting knife is risen to 2800rpm simultaneously, carries out cutting granulation.After granulation completes, the moist wood of formation is transferred in fluid bed and carry out drying, be about 2 hours drying time.Dried material first sieves according to particle requirement, remaining bulky grain and agglomerate are by particle shaping unit, the mesh sheet of adding suitable aperture as requested carries out particle shaping, and the particle after shaping through screening machine screening, finally obtains satisfactory Sucralose particle again.
Embodiment 4
Embodiment 1-3 is formed product that product and fluidized bed coating formed, sieve after initial crystalline product (requiring that granularity is close), jointly be placed in the baking oven of 70 DEG C, carry out Evaluation of Thermal Stability after 14.5 hours: the particle Sucralose effective content that present invention process is produced still keeps more than 90%, there is preferably heat endurance and the intensity of particle is good.
Claims (2)
1. the preparation method of a High thermal stability sucralose, it is characterized in that this preparation method is: join in Granulation Equipments by the crystallization Sucralose micro mist that the particle diameter D97 after pulverizing is less than 30um, while rotating speed is not less than 2500rpm high-speed stirred, by gunite system spray into water or concentration be 10%-50%w/w% aqueous solution of sucrose trichloride as binding agent, the feed postition of binding agent is evenly sprayed into by spraying system in the process of material dynamic motion; Then carry out granulation, granulation process temperature controls, within the scope of 20 DEG C-60 DEG C, to open cutting blade simultaneously, completes the cutting to agglomerate after Sucralose bonding, forms the granule that particle diameter has loose shape concrete dynamic modulus microstructure between 50um-800um; Obtain moisture after again this granule being put into drier drying and in particle shaping unit, carry out whole grain again after the material of 0.05%-0.2%w/w%, realize the control to grain diameter by the mesh sheet changing different pore size, finally the material after whole grain is sieved through screening machine; Sucralose particle appearance after screening is the nearly spherical particle of white, and good fluidity compared with initial crystalline Sucralose, has the angle of repose between 25 °-40 °; Particle size distribution range is narrow, and granule strength is comparatively large, is not easy to produce the undesirable dust of commercial Application because of broken;
Described binding agent is water or the aqueous solution of sucrose trichloride of concentration within the scope of 10%-50%w/w%, and wherein the weight ratio of binding agent and Sucralose micro mist is between 1:15-1:5.
2. the High thermal stability sucralose prepared of a preparation method as claimed in claim 1, it is characterized in that there are many hole shape structures the microstructure of this High thermal stability sucralose particle its inside compared with initial crystalline Sucralose, there is the loose bulk density between 0.4g/mL-0.8g/mL, and form oarse-grained initial superfines particle diameter D97 and be less than 30um.
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| 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 |
| 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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| 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 |
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