阅读说明：本技术 一种新型可控制粒度的蔗糖精制方法 (Novel sucrose refining method capable of controlling granularity ) 是由 唐波 彭立辉 于 2019-09-24 设计创作，主要内容包括：本发明公开了一种新型可控制粒度的蔗糖精制方法,包括将食用级蔗糖溶解脱色得精滤液,精滤液浓缩结晶得到蔗糖结晶,蔗糖结晶纯化干燥后得到药用级蔗糖晶粒。本发明创造性地采用晶种起晶和超声波刺激辅助起晶相结合的结晶方法,通过精确控制晶种添加时间、晶种的添加量、超声波频率、超声波刺激起晶时间及搅拌速率等参数,有效控制药用蔗糖晶体粒径,同时提高蔗糖结晶收率,实现药用蔗糖晶体粒径小,流动性好、溶解性好的特点,从而满足直压固体制剂中对药用蔗糖辅料的性能要求。(The invention discloses a novel sucrose refining method capable of controlling granularity, which comprises the steps of dissolving and decoloring edible sucrose to obtain refined filtrate, concentrating and crystallizing the refined filtrate to obtain sucrose crystals, purifying and drying the sucrose crystals to obtain medicinal sucrose crystal grains. The crystallization method combining seed crystal crystallization and ultrasonic wave stimulation assisted crystallization is creatively adopted, the grain size of the medicinal sucrose crystal is effectively controlled by accurately controlling the parameters of seed crystal adding time, seed crystal adding amount, ultrasonic frequency, ultrasonic wave stimulation crystallization time, stirring speed and the like, the sucrose crystallization yield is improved, and the characteristics of small grain size, good fluidity and good solubility of the medicinal sucrose crystal are realized, so that the performance requirements of a direct-compression solid preparation on the medicinal sucrose auxiliary material are met.)

1. A novel sucrose refining method with controllable particle size is characterized by comprising the following steps:

s1, dissolving and decoloring: dissolving edible sucrose in deionized water, adding a decolorizing agent, stirring at constant temperature, and filtering to obtain a fine filtrate;

s2, concentrating and crystallizing, namely stirring the fine filtrate obtained in the step S1, concentrating the fine filtrate to form sucrose viscous liquid with the sugar hammer degree of 87 ~ 92 degrees Bx, adding a certain amount of sucrose crystal seeds, stirring and dispersing, and simultaneously opening ultrasonic waves to stimulate the sucrose viscous liquid to crystallize to obtain crystallized liquid;

s3, separation and purification: separating the crystal liquid obtained in the step S2 to obtain coarse crystal grains, adding purified water into the coarse crystal grains, washing and stirring, and performing centrifugal separation to obtain crystal washing grains;

s4, drying and screening: and drying and screening the crystal washing crystal grains obtained in the step S3 to obtain medicinal sucrose crystal grains.

2. The novel sucrose refining method with controllable particle size as claimed in claim 1, wherein the temperature of dissolving food-grade sucrose in deionized water with constant temperature stirring is 75 ~ ℃ and the mass ratio of food-grade sucrose to deionized water is 2 ~: 1.

3. The method of claim 1, wherein the decolorizing agent of S1 is added in an amount of 0.05 ~ 0.1.1% of the food grade sucrose.

4. The novel sucrose refining process with controllable particle size as claimed in claim 1, wherein the decolorizing agent of S1 is injection grade pharmaceutical grade activated carbon.

5. The method as claimed in claim 1, wherein the concentration of the refined solution of S2 is carried out under reduced pressure at 70 ~ 80 deg.C and-0.09 ~ -0.07 MPa.

6. The method of claim 1, wherein the sucrose seed crystals of S2 are added in an amount of 0.1 ~ 0.3.3% by weight of food grade sucrose.

7. The method of claim 1, wherein the frequency of the ultrasonic-stimulated crystallization in S2 is 1500 ~ 1700Hz and the time of the ultrasonic-stimulated crystallization is 20 ~ 30 min.

8. The method of claim 1, wherein the stirring speed of S2 is 22 ~ 35 r/min.

9. The novel sucrose refining process with controllable particle size as claimed in claim 1, wherein the centrifugation top speed of S3 is 1000 ~ 1200 r/min.

10. The method of claim 1, wherein the drying temperature of the washed crystal grains of S4 is 63 ~ 67 ℃.

Technical Field

The invention relates to the technical field of sucrose refining, in particular to a novel sucrose refining method capable of controlling particle size.

Background

Sucrose has been used as a pharmaceutic adjuvant at home and abroad for hundreds of years, and has been used as food for a longer time. It can be used as excipient, correctant, coating agent, granulating agent, suspension, sweetener, filler, therapeutic agent, and tackifier. 85% syrup or aromatic syrup is used as correctant for oral liquid preparation, 50% -67% syrup is used as binder for wet granulation, sucrose powder can be used as dry binder, sucrose can be used as binder for dry tabletting, and can be used as filler and sweetener for chewable tablet and lozenge. Therefore, pharmaceutical sucrose is widely used in the production of solid preparations, is used in large amounts as an important filler and taste-improving agent, and when the tablet formulation contains a large amount of sugar, the hardness of the tablet can be increased but the degree of disintegration is deteriorated.

Medicinal grade sucrose belongs to adjuvant drugs, and sucrose cannot simultaneously have low bulk density, good fluidity, mixing property and excellent compressibility even being subjected to sufficient pulverization treatment due to its natural crystal structure. On one hand, common sucrose is in a natural crystallization mode, crystal particles are large in particle size, and although the flowability is good, the original particles exist in the tablet by direct tabletting, so that the appearance, dissolution, disintegration and other properties of the tablet are influenced; on the other hand, after sucrose is crushed into powdered sugar, although the solubility is improved, the crystal form of the product is damaged, the powdered sugar is easy to agglomerate, the flowability of the powdered sugar is poor, the uniform mixing is poor, the feeding cannot be smooth in the production of tablets, and the uniform tablets cannot be pressed. Therefore, even if the existing medicinal sucrose is widely applied, the existing medicinal sucrose can only be applied to the conventional non-direct-compression solid preparation production process in a sucrose tablet, cannot be applied to the direct-compression solid preparation process, and cannot ensure that the tablet has good dissolution and disintegration properties. There is a need to be able to prepare a pharmaceutical sucrose adjuvant with low bulk density, good flowability, uniformity and good compressibility.

Disclosure of Invention

The invention aims to solve the technical problems that the crystal form of sucrose powder prepared by the prior art is damaged and easy to agglomerate, the flowability of the powder is poor, and the uniform mixing is poor, and provides a novel sucrose refining method which has mild purification process conditions, is simple and feasible, has lower cost, and is environment-friendly and capable of controlling the granularity.

The purpose of the invention is realized by the following technical scheme:

a novel sucrose refining method with controllable particle size comprises the following steps:

s1, dissolving and decoloring: dissolving edible sucrose in deionized water, adding decolorizing agent, stirring at constant temperature, and filtering to remove solid impurities to obtain fine filtrate.

S2, concentrating and crystallizing, namely stirring the fine filtrate obtained in the step S1, concentrating until the sugar brix is 87 ~ 92 degrees Bx, adding a certain amount of sucrose crystal seeds, stirring and dispersing, and starting ultrasonic wave to stimulate and crystallize to obtain a crystalline liquid.

S3, separation and purification: and (4) separating the crystal liquid obtained in the step (S2) into coarse crystal grains and mother liquid, adding purified water into the coarse crystal grains, stirring, and performing centrifugal separation to obtain crystal washing grains and crystal washing liquid.

S4, drying and screening: and drying and screening the crystal washing crystal grains obtained in the step S3 to obtain medicinal sucrose crystal grains.

Further, the edible sucrose dissolved in the deionized water in S1 is stirred at a constant temperature of 75 ~ 85 ℃ and the mass ratio of the edible sucrose to the deionized water is 2 ~ 3: 1.

The S1 decolorant is added in an amount of 0.05 ~ 0.1.1% of the edible sucrose, adsorbs and removes pigments contained in the edible sucrose, preferably, the S1 decolorant is injection-grade medicinal activated carbon, and can adsorb and remove tiny particle impurities contained in the edible sucrose at the same time.

Further, the fine filtration liquid of S2 is concentrated under reduced pressure at 70 ~ 80 deg.C under-0.09 ~ -0.07 Mpa.

Solution crystallization is the process by which a substance is transformed from a liquid state to a crystalline state, which involves two phases, nucleation and crystal growth. The aim of seeking high crystal growth rate in an industrial crystallizer is to improve the production capacity of equipment, but the crystallization is rapid, the crystal nucleus quantity is difficult to control, the crystal nucleus production speed is not matched with the crystal nucleus growth speed, so that the size of the recrystallized crystals cannot be controlled, granular crystals with different sizes are easy to appear in the production process, the yield and the quality of finished products are influenced, and the requirement that sucrose powder is used as a solid preparation cannot be met by adopting a recrystallization mode for providing supersaturation to improve the growth rate of the crystals. Through scientific analysis and a large number of experiments, the method realizes the control of the grain size of the sucrose crystal by adopting ultrasonic waves and the stimulation crystallization added by the seed crystal and controlling the time for adding the seed crystal, the quality of the seed crystal, the frequency of the ultrasonic waves and the time for stimulating the crystallization by the ultrasonic waves.

Furthermore, experiments prove that the method provided by the invention has a better crystal growth speed for adding the seed crystal when the brix of the sucrose concentrated solution is 87 ~ 92 Bx, does not cause the grain size of the prepared crystal to be too large or too small, can improve the sucrose crystal yield and reduce the sucrose crystallization time, and meanwhile, the addition amount of the sucrose seed crystal in S2 is 0.1 ~ 0.3.3% of the quality of edible sucrose, the quantity of the seed crystal influences the generation of the crystal nucleus and the quality and yield of the crystal nucleus.

Furthermore, the frequency of ultrasonic wave stimulated crystallization of S2 is 1500 ~ Hz, the time of ultrasonic wave stimulated crystallization is 10 ~ min, in the process of crystal growth, ultrasonic wave is assisted, additional sound wave generates cavitation bubbles, the cavitation bubbles expand and grow, collapse quickly, when the bubbles collapse, a fast moving liquid flow is generated, and the liquid flow generates great impact force.

Further, the stirring speed of S2 is 22 ~ 35r/min, and preferably, the stirring speed of S2 is 28 r/min.

Furthermore, the highest speed of centrifugation is 1000 ~ 1200r/min, and the concentrated solution on the surface of the crystal is washed to prevent the crystal grains from caking and ensure better fluidity of powdered sugar.

Furthermore, the drying temperature of the crystal grain of the crystal washing of S4 is 63 ~ 67 ℃, the drying time is 60 ~ 150min, the grain diameter of the obtained sucrose crystal grain prepared by the method is 20 ~ 80 meshes, the purity reaches 99.9 ~ 99.99.99%, the fluidity is good, the moisture content is below 1.0%, and the product yield reaches 60 ~ 67%.

Compared with the prior art, the beneficial effects are:

the invention creatively adopts edible sucrose as a raw material to produce and prepare medicinal refined sucrose, scientifically designs purification steps, adopts dissolution and decoloration, reduced pressure concentration, seed crystal crystallization and ultrasonic stimulation crystallization, and separates and dries, and can obtain the sucrose auxiliary material which accords with Chinese pharmacopoeia by crystallization at a high speed under the condition of not using other organic solvents.

In the process of refining sucrose, the invention realizes effective control of the particle size of sucrose crystals by accurately controlling the parameters of the seed crystal addition time, the seed crystal addition amount, the ultrasonic frequency, the ultrasonic wave stimulated crystallization time, the stirring speed and the like, and simultaneously improves the sucrose crystallization yield, so that the prepared medicinal sucrose crystals have the characteristics of small particle size, good fluidity and good solubility, thereby meeting the performance requirements of a direct-compression solid preparation on medicinal sucrose auxiliary materials.

The method adopts the crystal seed crystallization and ultrasonic stimulation assisted crystallization modes, the grain diameter of the prepared sucrose crystal is 20 ~ 80 meshes (the optimal grain diameter range used by the solid preparation), the purity reaches 99 percent, and the yield is not lower than 60 percent.

Drawings

FIG. 1 is a flow chart of the preparation of the present invention;

FIG. 2 is a diagram of a production apparatus for refining sucrose with controllable particle size according to the present invention.

The device comprises a dissolving tank 1, a stirrer 2, a steam jacket 3, a filter screen 4, a titanium rod filter 5, a fine filter liquid tank 6, a concentration tank 7, a purified water inlet 8, a vacuum generator 9, an ultrasonic generator 10, a crystal seed dispenser 11, a centrifuge 12 and a fluidization vibrator 13.

Detailed Description

The following examples are further explained and illustrated, but the present invention is not limited in any way by the specific examples. Unless otherwise indicated, the methods and equipment used in the examples are conventional in the art and all materials used are conventional commercially available materials.

The required production equipment is provided by the following companies:

device name	Model number	Number of	Production plant
				Dissolving tank	5m3	1	Zibo bin combined chemical and equipment Limited
Titanium rod filter	9 core 30 inches	1	Hening hengtai filtration plant
				Fine filtering liquid tank	22m3	1	Ningxiang county culture of industry and trade Limited
Concentrating and crystallizing tank	3m3	1	Zibo bin combined chemical and equipment Limited
				Clean centrifugal machine	PSB800-100L	1	Zhang Jia City Chengjia machinery Co Ltd
Fluidized vibration bed dryer	ZGL-4.5×0.6	1	Changzhou new industry granulation drying equipment Co
				Vibrating screen	S4910-B	1	Xinxiangdongzi mechanical manufacturing Co Ltd