CN103131027B - Instant gellan gum and its preparation method - Google Patents
Instant gellan gum and its preparation method Download PDFInfo
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Abstract
本发明公开了一种速溶型结冷胶及其制备方法,以结冷胶粉体为起始原料,采用沸腾制粒干燥装置,将其制成速溶型结冷胶产品,该方法包括如下步骤:a)结冷胶粉体投料:将原料结冷胶粉体经净化的冷空气从沸腾制粒干燥装置的流化床底部引入,使原料处于沸腾状态;b)KCl水溶液湿润:喷入KCl水溶液使结冷胶粉体湿润并颗粒化;c)喷入结冷胶溶液:稀浓度的结冷胶溶液经雾化后,从流化床上部均匀喷入,用以包衣沸腾状态的原料结冷胶粉体;d)包衣;e)将所述颗粒产品干燥,以获得速溶型胶体基质。采用本发明方法制备的速溶型结冷胶用以解决现有生产中的粉体状结冷胶难以溶解、溶解过程中易形成“鱼眼”状团块,溶解时间慢以及粉尘飘逸的问题。
The invention discloses an instant gellan gum and a preparation method thereof. The gellan gum powder is used as a starting material, and a boiling granulation drying device is used to make an instant gellan gum product. The method comprises the following steps : a) Feeding of gellan gum powder: introduce the purified cold air from the bottom of the fluidized bed of the boiling granulation drying device to keep the raw material in a boiling state; b) Wetting the KCl aqueous solution: spray KCl The aqueous solution wets and granulates the gellan gum powder; c) Spraying the gellan gum solution: After the gellan gum solution of dilute concentration is atomized, it is sprayed evenly from the upper part of the fluidized bed to coat the boiling raw material Gellan gum powder; d) coating; e) drying the granular product to obtain an instant colloidal matrix. The instant gellan gum prepared by the method of the invention is used to solve the problems that the powdery gellan gum in the existing production is difficult to dissolve, easily forms "fish-eye"-like agglomerates during the dissolution process, has a slow dissolution time, and is free from dust.
Description
技术领域technical field
本发明涉及一种结冷胶,尤其涉及一种速溶型结冷胶;此外,本发明还涉及该速溶型结冷胶的制备方法。属于含有糖残基的化合物的制备。The invention relates to a gellan gum, in particular to an instant gellan gum; in addition, the invention also relates to a preparation method of the instant gellan gum. It belongs to the preparation of compounds containing sugar residues.
背景技术Background technique
结冷胶(Gellan Gum)是一种从水百合上分离所得的格兰氏阴性菌—伊乐藻假单胞杆菌(Pseudomonas elodea)对碳水化合物进行纯种培养发酵后,经提取精制而得的多糖胶质,近乎白色粉末,是一种新型的全透明的凝胶剂。现有技术中的结冷胶产品多为粉末状。Gellan Gum (Gellan Gum) is a Gram-negative bacterium isolated from water lilies—Pseudomonas elodea (Pseudomonas elodea) that is purified by fermentation of carbohydrates and extracted and refined. Polysaccharide colloid, almost white powder, is a new type of fully transparent gel. The gellan gum products in the prior art are mostly powdery.
结冷胶是一种高分子多糖,它的溶解过程与其他高聚物有共同之处。高聚物的溶解过程经历两个阶段,首先是溶剂分子渗入高聚物内部,使高聚物体积膨胀,即溶胀过程,然后才是高分子均匀分布在溶剂中,达到完全溶解。然而结冷胶在溶解过程中会有“鱼眼”(fish-eye)现象的产生:即胶在水中,颗粒表面由于水溶胀而形成胶质层,此时分子链并未形成能自由运动的无规线团状,胶质层的形成延缓并阻碍水分子向胶内部渗透,并且使颗粒之间发生胶结而成块状,形成表面是初期冻胶而内部却是干芯的大团块,使胶分子在水中溶胀与溶解速度降低,延长了溶解时间。Gellan gum is a high molecular polysaccharide, and its dissolution process has something in common with other high polymers. The dissolution process of the polymer goes through two stages. First, the solvent molecules penetrate into the polymer to expand the volume of the polymer, that is, the swelling process, and then the polymer is evenly distributed in the solvent to achieve complete dissolution. However, during the dissolution process of gellan gum, there will be a "fish-eye" phenomenon: that is, the glue is in water, and the surface of the particles forms a gelatinous layer due to water swelling. At this time, the molecular chains have not formed and can freely The movement of random coils, the formation of the colloidal layer delays and hinders the penetration of water molecules into the interior of the glue, and makes the particles cement together to form a block, forming a large group with an initial gel on the surface and a dry core inside. block, so that the swelling and dissolution speed of glue molecules in water is reduced, and the dissolution time is prolonged.
用户使用时,结冷胶溶液中出现小的团粒,“鱼眼”导致有些用户不得不增加过滤工序,将其过滤掉,造成结冷胶的浪费,也限制了其应用领域。另外,结冷胶粉体的生产和使用过程中粉尘对环境的污染,也是有待解决的问题。When users use it, small aggregates appear in the gellan gum solution, and "fish eyes" cause some users to have to increase the filtration process to filter them out, resulting in waste of gellan gum and limiting its application field. In addition, the pollution of dust to the environment during the production and use of gellan gum powder is also a problem to be solved.
为避免粉体状结冷胶在溶解过程中的结团现象,在配方及工艺允许的情况下,食品企业在使用过程中一般需先将结冷胶与一定比例的糖、盐等干物料一并混合,并且使用高速搅拌设备。但在实际应用中,不一定有干粉配料的配方,设备条件往往也会受到制约,况且即使与一定比例的干粉料预混也难以完全避免结团现象。In order to avoid the agglomeration of powdered gellan gum during the dissolution process, food companies generally need to combine gellan gum with a certain proportion of dry materials such as sugar and salt when the formula and process permit. And mix, and use high-speed mixing equipment. However, in practical applications, there is not necessarily a formula for dry powder ingredients, and equipment conditions are often restricted. Moreover, it is difficult to completely avoid agglomeration even if it is premixed with a certain proportion of dry powder.
由于结块的产生,许多厂家试图利用延长搅拌时间、提高搅拌速度的方式以达到结冷胶的充分溶解。但是,这种长时间的高速搅拌,不仅容易使大量空气裹入料液,影响最终产品的稳定性,同时也对许多不耐高剪切的配料产生非常不利的影响。Due to the generation of agglomeration, many manufacturers try to achieve the full dissolution of gellan gum by prolonging the stirring time and increasing the stirring speed. However, this long-term high-speed stirring not only easily causes a large amount of air to enter the feed liquid, affecting the stability of the final product, but also has a very adverse effect on many ingredients that are not resistant to high shear.
鉴于此,生产出快速溶解性的结冷胶对于结冷胶在食品工业中应用具有很大的推动作用。因此,亟需研发一种新型的速溶型结冷胶产品。In view of this, the production of rapidly soluble gellan gum has a great impetus for the application of gellan gum in the food industry. Therefore, urgently need to develop a kind of novel instant type gellan gum product.
发明内容Contents of the invention
本发明要解决的技术问题在于避免上述现有技术中的不足之处,而提供一种比表面积大、孔隙率高的速溶型结冷胶及其制备方法。本发明制备的速溶型结冷胶可以替代目前市售粉末状产品,解决现有技术中的结冷胶粉体(即粉末状结冷胶)难以溶解、溶解速度慢、溶解过程中易形成“鱼眼”状结团,溶解速度慢以及污染环境粉尘飞扬的问题。该速溶型结冷胶产品适用于市售酱料调味品、汤料、饮料、食品、药品行业使用。The technical problem to be solved by the present invention is to avoid the disadvantages of the above-mentioned prior art, and provide a kind of instant gellan gum with large specific surface area and high porosity and its preparation method. The instant gellan gum prepared by the present invention can replace the current commercially available powdered products, and solve the problem that the gellan gum powder (that is, powdered gellan gum) in the prior art is difficult to dissolve, the dissolution speed is slow, and the "" "fish-eye" agglomeration, slow dissolution rate and environmental dust pollution. The instant gellan gum product is suitable for use in the industries of sauces, seasonings, soups, beverages, food and pharmaceuticals.
通常的速溶型产品,基本上采用冷冻干燥或微胶囊化等手段来增加颗粒的比表面或对溶质在溶解前进行预乳化而使溶质快速分散。但从本质上该类只是溶质快速地分散在溶剂相中,通过乳化作用加快分散之后的溶解过程。The usual instant products basically use methods such as freeze-drying or microencapsulation to increase the specific surface of the particles or pre-emulsify the solute before dissolving to quickly disperse the solute. But in essence, this kind is just that the solute is quickly dispersed in the solvent phase, and the dissolution process after dispersion is accelerated through emulsification.
这些技术仅对在水中极容易分散或溶解的非粘性胶质有效。当将结冷胶加入水中时,它们在加入的过程中就立即开始增加粘性,这使得剩余的尚未加入的物质难以分散而不形成结块。These techniques are only effective for non-viscous colloids that disperse or dissolve very easily in water. When gellan gums are added to water, they immediately start to gain viscosity as they are added, making it difficult for the remaining material that has not been added to disperse without forming clumps.
本发明通过研究,采用各种手段使结冷胶在溶解时,使表面已溶胀的胶分子较快地脱离胶颗粒形成自由运动的无规线团状,从而达到分子水平的速溶目的,宏观表现为样品的迅速溶解,溶液粘度的迅速增加。Through research, the present invention adopts various means to make gellan gum dissolve, so that the swollen glue molecules on the surface are separated from the glue particles quickly to form free-moving random coils, so as to achieve the purpose of instant dissolution at the molecular level. For the rapid dissolution of the sample, the viscosity of the solution increases rapidly.
为解决上述技术问题,本发明提供一种速溶型结冷胶的制备方法,以结冷胶粉体(即粉末状结冷胶)为起始原料,采用沸腾制粒干燥装置,将其制成速溶型结冷胶产品,该方法包括如下操作步骤:In order to solve the above-mentioned technical problems, the present invention provides a preparation method of instant gellan gum, which uses gellan gum powder (i.e. powdered gellan gum) as the starting material and adopts a boiling granulation drying device to make it into Instant type gellan gum product, the method comprises the following steps:
a)结冷胶粉体投料:将原料结冷胶粉体经净化的冷空气从沸腾制粒干燥装置的流化床底部引入,使原料结冷胶粉体处于沸腾状态;a) Feeding of gellan gum powder: introduce the purified cold air from the bottom of the fluidized bed of the fluidized granulation drying device to keep the raw material gellan gum powder in a boiling state;
b)KCl水溶液湿润:喷入KCl水溶液使原料结冷胶粉体湿润并颗粒化;b) Wetting of KCl aqueous solution: Spray KCl aqueous solution to wet and granulate the raw material gellan gum powder;
c)喷入结冷胶溶液:稀浓度的结冷胶溶液经雾化后,从流化床上部均匀喷入,用以包衣沸腾状态的原料结冷胶粉体;c) Spraying gellan gum solution: after the gellan gum solution of dilute concentration is atomized, it is sprayed evenly from the upper part of the fluidized bed to coat the raw material gellan gum powder in boiling state;
d)包衣:经高压喷枪雾化,形成的雾状液滴,喷洒于流化床内的结冷胶粉体,借助结冷胶本身的粘性,遇水后碰撞粘合形成小颗粒,在沸腾制粒过程中,颗粒逐渐增大,最终形成所需要的多微孔球状包衣的颗粒;d) Coating: Atomized by a high-pressure spray gun, the mist-like droplets formed are sprayed on the gellan gum powder in the fluidized bed. With the help of the viscosity of the gellan gum itself, it collides with water to form small particles. During the boiling granulation process, the granules gradually increase and finally form the required microporous spherical coated granules;
e)将所述颗粒产品干燥,以获得速溶型胶体基质。e) drying the granular product to obtain an instant colloidal matrix.
优选地,在步骤e)之后还包括以下步骤:Preferably, after step e), the following steps are also included:
f)用分级筛筛分或整粒机整粒的方法处理所述颗粒产品至合适的粒度大小;按照速溶大小分级要求,分别过相应目数的筛子,筛去少量未成粒细粉和大颗粒;也可以使用整粒机,获得所期望的颗粒度;f) Process the granule product to a suitable particle size by sieving with a grading sieve or granulating with a granulator; according to the instant size grading requirements, pass through sieves with corresponding meshes to remove a small amount of ungranulated fine powder and large particles ; You can also use a granulator to obtain the desired particle size;
g)质量检验,合格后包装入库。g) Quality inspection, packaging and storage after passing the test.
优选地,在步骤a)中,所述结冷胶粉体的投料量为采用的沸腾制粒干燥设备生产能力的40%~80%。Preferably, in step a), the feeding amount of the gellan gum powder is 40%-80% of the production capacity of the fluidized granulation drying equipment used.
优选地,在步骤a)中,所述结冷胶粉体是高酰基结冷胶,或者低酰基结冷胶。Preferably, in step a), the gellan gum powder is high acyl gellan gum or low acyl gellan gum.
优选地,在步骤b)中,将0.1%~3%质量百分比浓度的KCl溶液雾化后,从流化床上部均匀喷入,喷洒时间20-60分钟,雾化压力0.25-0.5MPa。Preferably, in step b), after atomizing the KCl solution with a concentration of 0.1% to 3% by mass, it is sprayed evenly from the upper part of the fluidized bed, the spraying time is 20-60 minutes, and the atomization pressure is 0.25-0.5 MPa.
优选地,在步骤c)中,所述结冷胶溶液的用量为投入原料结冷胶粉体重量的5%~30%,喷洒时间控制在20~120分钟,雾化压力为0.3MPa~0.6MPa;所述结冷胶溶液的浓度为0.05%~0.2%(该结冷胶溶液的浓度是指结冷胶占结冷胶水溶液的质量百分比浓度)。Preferably, in step c), the dosage of the gellan gum solution is 5% to 30% of the weight of the input raw material gellan gum powder, the spraying time is controlled at 20 to 120 minutes, and the atomization pressure is 0.3MPa to 0.6 MPa; the concentration of the gellan gum solution is 0.05% to 0.2% (the concentration of the gellan gum solution refers to the mass percentage concentration of gellan gum in the gellan gum aqueous solution).
优选地,在步骤e)中,当颗粒粒径达到工艺要求后,停止喷入溶液,热风继续通入,并保持温度60℃~90℃,继续干燥至水分含量≤13%,干燥时间20~120分钟。Preferably, in step e), when the particle size reaches the process requirement, stop spraying the solution, continue to feed hot air, keep the temperature at 60°C-90°C, and continue drying until the moisture content is ≤13%, and the drying time is 20- 120 minutes.
优选地,在步骤b)和步骤c)之间增加如下步骤:湿润后粉体形成微粒后,经净化过的冷空气经蒸汽预热后,热风温度60~90℃,蒸汽压力0.4MPa~0.8MPa。Preferably, the following steps are added between step b) and step c): After the wetted powder forms particles, the purified cold air is preheated by steam, the temperature of the hot air is 60-90°C, and the steam pressure is 0.4MPa-0.8 MPa.
此外,本发明还提供一种采用上述方法制得的速溶型结冷胶。In addition, the present invention also provides an instant gellan gum prepared by the above method.
本发明的速溶型结冷胶的制备方法,不添加其他成分,利用物料本身特性制粒,不改变物料本身性质,通过物理形态改变达到改善其分散水合性能的目的,提高结冷胶的分散水合速度,不但解决了结冷胶结团的技术难题,而且溶解速度快速增加,显著改善了其应用性能。The preparation method of instant gellan gum of the present invention does not add other ingredients, uses the characteristics of the material itself to granulate, does not change the properties of the material itself, and achieves the purpose of improving its dispersion and hydration performance through physical form changes, and improves the dispersion and hydration of gellan gum. The speed not only solves the technical problem of gellan gum agglomeration, but also increases the dissolution rate rapidly, which significantly improves its application performance.
利用本发明的方法制备的速溶型结冷胶产品具有疏松多孔状结构,相比粉末结冷胶具有更好的分散性和更快的水合速度,避免了普通粉状结冷胶在使用过程中由于来不及分散导致的结团现象。The instant gellan gum product prepared by the method of the present invention has a loose and porous structure, has better dispersion and faster hydration speed than powdered gellan gum, and avoids the use of ordinary powdered gellan gum. Agglomeration caused by too late to disperse.
一些技术,如使用具有宽的HLB(亲水和亲脂平衡)范围的表面活性剂和润湿剂的包衣和团聚技术,用于“难以分散的”胶质。但仅在某种程度上改善了粘性的快速溶胀的胶质的分散性,其缺点:①不可能低速混合搅拌而不形成结块;②许多润湿剂和表面活性剂增加了结冷胶溶液的透明度;③润湿剂和表面活性剂会带来异味。Some techniques, such as coating and agglomeration techniques using surfactants and wetting agents with a wide HLB (hydrophilic and lipophilic balance) range, are used for "difficult to disperse" gums. However, the dispersibility of viscous fast-swelling colloids is only improved to some extent, and its disadvantages are: ①It is impossible to mix and stir at low speed without forming agglomerates; ②Many wetting agents and surfactants increase the gellan gum solution. Transparency; ③ wetting agents and surfactants will bring odor.
速溶型结冷胶可以在低剪切条件下分散,可以减少高速分散设备投入,有助于减少在搅拌过程中的空气裹入,对于体系稳定性,尤其是乳化体系的稳定性极为有利。不仅应用上方便,而且节省高速搅拌设备的投资。Instant gellan gum can be dispersed under low-shear conditions, which can reduce the investment in high-speed dispersion equipment and help reduce air entrainment during stirring, which is extremely beneficial to system stability, especially the stability of emulsified systems. It is not only convenient in application, but also saves investment in high-speed mixing equipment.
本发明与现有技术相比,具有如下有益效果:Compared with the prior art, the present invention has the following beneficial effects:
1.提供了一种比表面积大、孔隙率高的速溶型结冷胶的制备方法。制备的速溶型结冷胶解决现有技术中的粉体型结冷胶溶解速度慢、溶解过程中结团,以及粉尘污染的问题。1. A preparation method of instant gellan gum with large specific surface area and high porosity is provided. The prepared instant gellan gum solves the problems of slow dissolution speed, agglomeration during the dissolution process and dust pollution of the powder type gellan gum in the prior art.
2.提供了分散性好、溶解快的速溶型新产品,解决了结冷胶在应用中的结团问题,改善其应用性能,提高原料利用率,节省时间。2. Provide a new instant product with good dispersibility and fast dissolution, which solves the agglomeration problem of gellan gum in application, improves its application performance, improves the utilization rate of raw materials, and saves time.
3.本发明速溶型结冷胶达到完全水合的时间大大缩短(如图1所示),30秒内完全分散,3分钟即可基本达到完全水合,呈均匀溶胶状态,而普通粉状结冷胶则结团未完全溶解,至少需要30分钟才能基本水合完全。在盐溶液和糖溶液中这种差别更加明显。3. The time for the instant gellan gum of the present invention to reach complete hydration is greatly shortened (as shown in Figure 1), it is completely dispersed within 30 seconds, and it can basically reach complete hydration in 3 minutes, in a state of uniform sol, while ordinary powdery gellan gum The glue is agglomerated and not completely dissolved, and it takes at least 30 minutes to be completely hydrated. This difference is even more pronounced in saline and sugar solutions.
4.在蔗糖溶液中(如图2所示),本发明速溶型结冷胶只需要1分钟左右即可完全水合达到平衡粘度。而普通粉状结冷胶粘度释放缓慢,在分散20分钟后,才能水合完全,基本达到最高粘度。4. In the sucrose solution (as shown in FIG. 2 ), the instant gellan gum of the present invention can be completely hydrated to reach the equilibrium viscosity in about 1 minute. The viscosity of ordinary powdered gellan gum releases slowly, and it can be completely hydrated after dispersing for 20 minutes, and basically reaches the highest viscosity.
5.速溶型结冷胶与普通粉状结冷胶相比具有更快的分散水合速率,不易结团,水合充分。在实际应用中,能大大节省时间,使投料充分利用从而减少物料的浪费,提高原料利用的有效性。5. Compared with ordinary powdered gellan gum, instant gellan gum has a faster dispersion and hydration rate, is not easy to agglomerate, and has sufficient hydration. In practical application, it can greatly save time, make full use of feeding materials, reduce material waste, and improve the effectiveness of raw material utilization.
6.本发明还可以避免粉状结冷胶使用中的扬尘问题,从而改善了结冷胶的使用环境。6. The present invention can also avoid the problem of raising dust in the use of powdery gellan gum, thereby improving the use environment of gellan gum.
附图说明Description of drawings
本发明下面将结合附图做进一步详述:The present invention will be described in further detail below in conjunction with accompanying drawing:
图1是普通粉状结冷胶和本发明速溶型结冷胶在水中分散水合速率比较示意图。Figure 1 is a schematic diagram of the comparison of the dispersion and hydration rates of ordinary powdered gellan gum and the instant gellan gum of the present invention in water.
图2是普通粉状结冷胶与本发明速溶型结冷胶在蔗糖溶液中的分散水合速率比较示意图。Fig. 2 is a schematic diagram showing the comparison of dispersion and hydration rates of ordinary powdered gellan gum and the instant gellan gum of the present invention in sucrose solution.
在图1和图2中,横坐标代表时间(单位:min(分钟)),纵坐标代表粘度(单位:CP(厘泊))。In Figure 1 and Figure 2, the abscissa represents time (unit: min (minute)), and the ordinate represents viscosity (unit: CP (centipoise)).
具体实施方式Detailed ways
实施例1Example 1
以结冷胶粉体为起始原料,采用沸腾制粒干燥机,操作步骤如下:Using gellan gum powder as the starting material, using a boiling granulation dryer, the operation steps are as follows:
①.结冷胶粉体投料①. Gellan gum powder feeding
原料结冷胶粉体投入流化床,投料量为2公斤。净化过的空气经从沸腾制粒干燥装置的流化床底部引入,使原料结冷胶粉体处于沸腾状态;The raw material gellan gum powder is put into the fluidized bed, and the feeding amount is 2 kg. The purified air is introduced from the bottom of the fluidized bed of the fluidized granulation drying device, so that the raw material gellan gum powder is in a boiling state;
②.喷入KCl溶液②. Spray KCl solution
用蠕动泵,将0.2%质量百分比浓度的KCl溶液雾化后,从流化床上部均匀喷入,喷洒时间30分钟,雾化压力0.4MPa;Use a peristaltic pump to atomize the KCl solution with a concentration of 0.2% by mass, and spray it evenly from the upper part of the fluidized bed. The spraying time is 30 minutes, and the atomization pressure is 0.4MPa;
③.喷入结冷胶溶液③. Spray gellan gum solution
稀浓度的结冷胶溶液经雾化后,从流化床上部均匀喷入,用以包衣沸腾状态的原料结冷胶粉体;所述结冷胶溶液的用量为投入原料结冷胶粉体重量的5%,喷洒时间控制在20分钟,雾化压力为0.3MPa;所述结冷胶溶液的浓度为0.05%。After the gellan gum solution of dilute concentration is atomized, it is evenly sprayed from the upper part of the fluidized bed to coat the raw material gellan gum powder in a boiling state; 5% of the body weight, the spraying time is controlled at 20 minutes, and the atomization pressure is 0.3MPa; the concentration of the gellan gum solution is 0.05%.
④.沸腾制粒,包衣④. Boiling granulation, coating
经高压喷枪雾化,形成的雾状液滴,喷洒于流化床上的结冷胶粉体,借助结冷胶本身的粘性,遇水后碰撞粘合形成小速溶,在沸腾制粒过程中,速溶逐渐增大,最终形成所需要的多微孔球状包衣的颗粒;Atomized by a high-pressure spray gun, the formed mist-like droplets are sprayed on the gellan gum powder on the fluidized bed. With the help of the viscosity of the gellan gum itself, it collides with water and forms a small instant solution. During the boiling granulation process , the instant solution gradually increases, and finally forms the required microporous spherical coated particles;
⑤.干燥⑤. Drying
当颗粒粒径达到工艺要求后,停止喷KCl溶液,引入热风,同时通入0.1%的结冷胶溶液,并保持温度60℃,继续干燥至水分含量≤13%,干燥时间60分钟;When the particle size reaches the process requirements, stop spraying KCl solution, introduce hot air, and at the same time pass 0.1% gellan gum solution, and keep the temperature at 60°C, continue drying until the moisture content is ≤13%, and the drying time is 60 minutes;
⑥.筛分⑥. Screening
按照速溶大小分级要求,分别过相应目数的筛子,筛去少量未成粒细粉和大速溶;According to the classification requirements of instant dissolving size, pass through sieves with corresponding meshes respectively, and sieve out a small amount of ungranulated fine powder and large instant dissolving;
⑦.质量检验,合格后包装入库。⑦. Quality inspection, packaging and storage after passing the test.
实施例2Example 2
以结冷胶粉体为起始原料,采用沸腾制粒干燥机,操作步骤如下:Using gellan gum powder as the starting material, using a boiling granulation dryer, the operation steps are as follows:
①.结冷胶粉体投料①. Gellan gum powder feeding
原料结冷胶粉体投入流化床,投料量为2公斤。净化过的空气经从沸腾制粒干燥装置的流化床底部引入,使原料结冷胶粉体处于沸腾状态;The raw material gellan gum powder is put into the fluidized bed, and the feeding amount is 2 kg. The purified air is introduced from the bottom of the fluidized bed of the fluidized granulation drying device, so that the raw material gellan gum powder is in a boiling state;
②.喷入KCl溶液②. Spray KCl solution
用蠕动泵,将0.2%质量百分比浓度的KCl溶液雾化后,从流化床上部均匀喷入,喷洒时间20分钟,雾化压力0.5MPa;Use a peristaltic pump to atomize the KCl solution with a concentration of 0.2% by mass, and spray it evenly from the upper part of the fluidized bed. The spraying time is 20 minutes, and the atomization pressure is 0.5MPa;
③.喷入结冷胶溶液③. Spray gellan gum solution
稀浓度的结冷胶溶液经雾化后,从流化床上部均匀喷入,用以包衣沸腾状态的原料结冷胶粉体;所述结冷胶溶液的用量为投入原料结冷胶粉体重量的30%,喷洒时间控制在120分钟,雾化压力为0.6MPa;所述结冷胶溶液的浓度为0.2%。After the gellan gum solution of dilute concentration is atomized, it is evenly sprayed from the upper part of the fluidized bed to coat the raw material gellan gum powder in a boiling state; 30% of the body weight, the spraying time is controlled at 120 minutes, and the atomization pressure is 0.6MPa; the concentration of the gellan gum solution is 0.2%.
④.沸腾制粒,包衣:④. Boiling granulation, coating:
经高压喷枪雾化,形成的雾状液滴,喷洒于流化床上的结冷胶粉体,借助结冷胶本身的粘性,遇水后碰撞粘合形成小速溶,在沸腾制粒过程中,速溶逐渐增大,最终形成所需要的多微孔球状包衣的颗粒;Atomized by a high-pressure spray gun, the formed mist-like droplets are sprayed on the gellan gum powder on the fluidized bed. With the help of the viscosity of the gellan gum itself, it collides with water and forms a small instant solution. During the boiling granulation process , the instant solution gradually increases, and finally forms the required microporous spherical coated particles;
⑤.干燥⑤. Drying
当颗粒粒径达到工艺要求后,停止喷KCl溶液,引入热风,同时通入0.1%的结冷胶溶液,并保持温度90℃,继续干燥至水分含量≤13%,干燥时间20分钟;When the particle size reaches the process requirements, stop spraying KCl solution, introduce hot air, and at the same time pass 0.1% gellan gum solution, and keep the temperature at 90°C, continue drying until the moisture content is ≤13%, and the drying time is 20 minutes;
⑥.筛分⑥. Screening
按照速溶大小分级要求,分别过相应目数的筛子,筛去少量未成粒细粉和大速溶;According to the classification requirements of instant dissolving size, pass through sieves with corresponding meshes respectively, and sieve out a small amount of ungranulated fine powder and large instant dissolving;
⑦.质量检验,合格后包装入库。⑦. Quality inspection, packaging and storage after passing the test.
实施例3Example 3
以结冷胶粉体为起始原料,采用沸腾制粒干燥机,操作步骤如下:Using gellan gum powder as the starting material, using a boiling granulation dryer, the operation steps are as follows:
①.结冷胶粉体投料①. Gellan gum powder feeding
原料结冷胶粉体投入流化床,投料量为2公斤。净化过的空气经从沸腾制粒干燥装置的流化床底部引入,使原料结冷胶粉体处于沸腾状态;The raw material gellan gum powder is put into the fluidized bed, and the feeding amount is 2 kg. The purified air is introduced from the bottom of the fluidized bed of the fluidized granulation drying device, so that the raw material gellan gum powder is in a boiling state;
②.喷入KCl溶液②. Spray KCl solution
用蠕动泵,将0.2%质量百分比浓度的KCl溶液雾化后,从流化床上部均匀喷入,喷洒时间60分钟,雾化压力0.25MPa;Use a peristaltic pump to atomize the KCl solution with a concentration of 0.2% by mass, and spray it evenly from the upper part of the fluidized bed. The spraying time is 60 minutes, and the atomization pressure is 0.25MPa;
③.喷入结冷胶溶液③. Spray gellan gum solution
稀浓度的结冷胶溶液经雾化后,从流化床上部均匀喷入,用以包衣沸腾状态的原料结冷胶粉体;所述结冷胶溶液的用量为投入原料结冷胶粉体重量的20%,喷洒时间控制在90分钟,雾化压力为0.4MPa;所述结冷胶溶液的浓度为0.1%。After the gellan gum solution of dilute concentration is atomized, it is evenly sprayed from the upper part of the fluidized bed to coat the raw material gellan gum powder in a boiling state; 20% of the body weight, the spraying time is controlled at 90 minutes, and the atomization pressure is 0.4MPa; the concentration of the gellan gum solution is 0.1%.
④.沸腾制粒,包衣:④. Boiling granulation, coating:
经高压喷枪雾化,形成的雾状液滴,喷洒于流化床上的结冷胶粉体,借助结冷胶本身的粘性,遇水后碰撞粘合形成小速溶,在沸腾制粒过程中,速溶逐渐增大,最终形成所需要的多微孔球状包衣的颗粒;Atomized by a high-pressure spray gun, the formed mist-like droplets are sprayed on the gellan gum powder on the fluidized bed. With the help of the viscosity of the gellan gum itself, it collides with water and forms a small instant solution. During the boiling granulation process , the instant solution gradually increases, and finally forms the required microporous spherical coated particles;
⑤.干燥⑤. Drying
当颗粒粒径达到工艺要求后,停止喷KCl溶液,引入热风,同时通入0.1%的结冷胶溶液,并保持温度70℃,继续干燥至水分含量≤13%,干燥时间120分钟;When the particle size reaches the process requirements, stop spraying KCl solution, introduce hot air, and at the same time pass 0.1% gellan gum solution, and keep the temperature at 70°C, continue drying until the moisture content is ≤13%, and the drying time is 120 minutes;
⑥.筛分⑥. Screening
按照速溶大小分级要求,分别过相应目数的筛子,筛去少量未成粒细粉和大速溶;According to the classification requirements of instant dissolving size, pass through sieves with corresponding meshes respectively, and sieve out a small amount of ungranulated fine powder and large instant dissolving;
⑦.质量检验,合格后包装入库。⑦. Quality inspection, packaging and storage after passing the test.
以下通过试验例对本发明的有益效果作进一步的阐述:Beneficial effects of the present invention are further elaborated below by test example:
测试说明Test instruction
用测试粘度的方法,在烧杯中使用用搅拌器搅拌以测试最终产品在水中的分散和溶解。用下述的测试步骤和方法:To test the viscosity, use a stirrer in a beaker to test the dispersion and dissolution of the final product in water. Use the following test steps and methods:
试验例一Test example one
1、在600mL烧杯中称量394g的水,在天平上称量6g的速溶型结冷胶,对比实验用普通粉状结冷胶6g;1. Weigh 394g of water in a 600mL beaker, weigh 6g of instant gellan gum on a balance, and use 6g of ordinary powdered gellan gum for comparison experiments;
2、将搅拌浆置于烧杯中的液面下中部偏上;2. Place the stirring paddle in the beaker below the liquid surface and above the middle;
3、启动电源,初始转速为400RPM,在5秒内将粉体匀速倒入水中,并启动计时器;根据粘度加大转速使溶液整体搅动;3. Start the power supply, the initial speed is 400RPM, pour the powder into the water at a constant speed within 5 seconds, and start the timer; increase the speed according to the viscosity to stir the solution as a whole;
4、准确地在0.5、1、2、3、5、10、20和30分钟时在Brookfield粘度计中以60RPM测量粘度。在每次粘度测量之后将溶液放回到搅拌器中;4. Measure the viscosity in a Brookfield viscometer at 60 RPM at exactly 0.5, 1, 2, 3, 5, 10, 20 and 30 minutes. Return the solution to the mixer after each viscosity measurement;
5、观察溶液状态。5. Observe the state of the solution.
测试结果见图1,普通粉状结冷胶和本发明速溶型结冷胶在水中分散水合速率比较示意图。从图1可以看出,在400rpm转速下,本发明速溶型结冷胶在5分钟内几乎达到最大粘度,而普通粉状结冷胶在前5分钟内粘度几乎没有很大变化,在20分钟内才达到最大粘度的80%。The test results are shown in Figure 1, which is a schematic diagram of the comparison of the dispersion and hydration rates of ordinary powdered gellan gum and the instant gellan gum of the present invention in water. As can be seen from Fig. 1, under the 400rpm rotating speed, the instant gellan gum of the present invention almost reaches the maximum viscosity in 5 minutes, while the viscosity of ordinary powdered gellan gum hardly changes in the first 5 minutes, and in 20 minutes 80% of the maximum viscosity is reached.
现象:当速溶型结冷胶倒入烧杯后,在2~5秒内即可分散于整个溶液中,外观表现为肉眼可见的细微晶体小球在溶液中旋转,溶液并开始变稠。普通粉末型结冷胶则形成块状在溶液中旋转,当粘度上升到800cp时,仍有少量团状物。可见,与普通粉末型结冷胶相比,本发明速溶型结冷胶达到完全水合的时间大大缩短,30秒内完全分散,3分钟即可基本达到完全水合,呈均匀溶胶状态。Phenomenon: After the instant gellan gum is poured into the beaker, it can be dispersed in the whole solution within 2 to 5 seconds. The appearance is that the fine crystal balls visible to the naked eye are rotating in the solution, and the solution begins to thicken. Ordinary powder-type gellan gum forms lumps and rotates in the solution. When the viscosity rises to 800cp, there are still a small amount of lumps. It can be seen that compared with ordinary powdered gellan gum, the time for the instant gellan gum of the present invention to reach complete hydration is greatly shortened, it can be completely dispersed within 30 seconds, and can basically reach complete hydration in 3 minutes, showing a uniform sol state.
试验例二Test example two
1、在600mL烧杯中称量388g的水,在天平上称量6g的速溶型结冷胶和6g蔗糖,对比实验用普通粉状结冷胶6g和蔗糖6g;1. Weigh 388g of water in a 600mL beaker, weigh 6g of instant gellan gum and 6g of sucrose on a balance, and use 6g of ordinary powdered gellan gum and 6g of sucrose for comparison experiments;
2、将搅拌浆置于烧杯中的液面下中部偏上;2. Place the stirring paddle in the beaker below the liquid surface and above the middle;
3、启动电源,初始转速为400RPM,在5秒内将粉体匀速倒入水中,并启动计时器;根据粘度加大转速使溶液整体搅动;3. Start the power supply, the initial speed is 400RPM, pour the powder into the water at a constant speed within 5 seconds, and start the timer; increase the speed according to the viscosity to stir the solution as a whole;
4、准确地在0.5、1、2、3、5、10、20和30分钟时在Brookfield粘度计中以60RPM测量粘度。在每次粘度测量之后将溶液放回到搅拌器中;4. Measure the viscosity in a Brookfield viscometer at 60 RPM at exactly 0.5, 1, 2, 3, 5, 10, 20 and 30 minutes. Return the solution to the mixer after each viscosity measurement;
5、观察溶液状态。5. Observe the state of the solution.
测试结果见图2,普通粉状结冷胶与本发明速溶型结冷胶在蔗糖溶液中的分散水合速率比较示意图。从图2可以看出,在400rpm转速下,本发明速溶型结冷胶在5分钟即可全部溶解,在2分钟内即能达到最大粘度。而普通粉状结冷胶虽然比没加糖有所改善,但粘度形成效果不是很明显。在蔗糖溶液中,本发明速溶型结冷胶只需要1分钟左右即可完全水合达到平衡粘度。而普通粉状结冷胶粘度释放缓慢,在分散20分钟后,才能水合完全,基本达到最高粘度。The test results are shown in Figure 2, which is a schematic diagram of the comparison of the dispersion and hydration rates of ordinary powdered gellan gum and the instant gellan gum of the present invention in sucrose solution. As can be seen from Fig. 2, under the rotating speed of 400rpm, the instant gellan gum of the present invention can be completely dissolved in 5 minutes, and can reach the maximum viscosity in 2 minutes. Although ordinary powdered gellan gum is better than that without sugar, the viscosity formation effect is not very obvious. In a sucrose solution, the instant gellan gum of the present invention can be completely hydrated to reach an equilibrium viscosity in about 1 minute. The viscosity of ordinary powdered gellan gum releases slowly, and it can be completely hydrated after dispersing for 20 minutes, and basically reaches the highest viscosity.
现象:含糖速溶型结冷胶倒入烧杯过程中,既可分散于整个溶液中,肉眼可见的细微晶体小球在溶液中旋转中溶解,溶液变稠。含糖普通粉末型结冷胶在溶解过程中虽然分散性有改善,但仍有“鱼眼”状团块。Phenomenon: When the sugar-containing instant gellan gum is poured into the beaker, it can be dispersed in the whole solution, and the fine crystal balls visible to the naked eye dissolve in the solution, and the solution becomes thick. Although the dispersibility of sugar-containing common powder gellan gum is improved during the dissolution process, there are still "fish-eye" lumps.
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EP1853658B1 (en) * | 2005-03-03 | 2009-02-18 | Wacker Chemie AG | Use of silicon oxide compounds as free-flow agents in the production of solid polyvinyl acetate resins |
CN101595190A (en) * | 2006-12-28 | 2009-12-02 | 巴斯夫欧洲公司 | Be used to polish the composition on the surface of making by silicon-dioxide |
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CN1687437A (en) * | 2005-03-25 | 2005-10-26 | 张禹 | Method of high post extraction of acyl Gellan |
CN101062957A (en) * | 2006-04-24 | 2007-10-31 | 上海众伟生化有限公司 | Gellan gum without organic solvent and production technique thereof |
CN101595190A (en) * | 2006-12-28 | 2009-12-02 | 巴斯夫欧洲公司 | Be used to polish the composition on the surface of making by silicon-dioxide |
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