CN102106870B - Method for preparing high-density calcium carbonate granules - Google Patents
Method for preparing high-density calcium carbonate granules Download PDFInfo
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- CN102106870B CN102106870B CN200910199344.9A CN200910199344A CN102106870B CN 102106870 B CN102106870 B CN 102106870B CN 200910199344 A CN200910199344 A CN 200910199344A CN 102106870 B CN102106870 B CN 102106870B
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Abstract
The invention discloses a method for preparing high-density calcium carbonate granules, which comprises the following steps of: A, adding calcium carbonate powder into a mixing granulator; B, mixing a bonding agent and water, controlling the temperature to be below a set value, spraying the mixed bonding agent and water into the mixing granulator for granulating; C, sorting the granules; D, drying the granules processed in the step C; E, dividing the granules into granular section with different sizes by sieving; and F, mixing. The high-density calcium carbonate granules prepared by the method have uniform distribution of granularity, concentrated granularity and high liquidity, so in the tabletting stage, the tablet weight is uniform, the compressibility is high; simultaneously, the loss of a machine can be prolonged, and the service life of the machine can be prolonged.
Description
Technical field
The invention belongs to inorganic chemicals industry technical field, relate to a kind of high-density calcium carbonate particles, particularly relate to a kind of manufacture method of high-density calcium carbonate particles.
Background technology
Calcium is the metallic element that people's in-vivo content is maximum, about has 1200 grams, is also one of element the most easily lacked.Wherein 99% be formed at skeleton, 1% is present in blood soft tissue.Whether calcium deficiency is relevant with two reasons for human body: one is Peak Bone Mass, and namely when one's mid-30s, human body bone amount reaches calcium content during most high bone mass in life, determines primarily of inherited genetic factors, factor of replenishing the calcium and exercise factors; Two is calcium loss situations, determined by the supplementing of calcium, number of dropouts and living habit, as too high addicted to tobacco and wine, coffee, tea, cola, Salt intake, eat meat less or eats the loss that too many meat all can cause calcium.
Edible calsium supplement generally adopts the calcium carbonate from natural origin, comprises limestone and Concha Ostreae.Recommend according to Chinese Soclety of Nutrition, the magnitude of recruitment of adult's one day calcium is at 600mg.Therefore, the instructions of taking supplementing calcium preparation takes the calcium tablet of a slice containing 600mg calcium general every day.Even if but like this, most of calcium tablet is still very large, dysphagia or make us uncomfortable.Therefore, occurred that some reduce the method for tablet sizes.But the method for existing reduction tablet sizes does not also make the density of calcium carbonate granule reach satisfactory value, and the present invention is improved.
Summary of the invention
Technical problem to be solved by this invention is: the manufacture method providing a kind of high-density calcium carbonate particles, effectively can improve the density of tablet.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A manufacture method for high-density calcium carbonate particles, the method comprises the steps:
A, calcium carbonate powder is joined in mixer-granulator;
B, binding agent and water are sized mixing, temperature controls under setting value, the binding agent after sizing mixing and water is sprayed in mixer-granulator and granulates;
C, granulate step;
D, dried is carried out to the granule after step C process;
E, by screening, granule is divided into the granule section varied in size;
F, blend step.
As a preferred embodiment of the present invention, in described step C, before granulate, carry out pre-drying step, then granulate.
As a preferred embodiment of the present invention, the binding agent in described step B is pregelatinized Starch.
As a preferred embodiment of the present invention, the percentage by weight of calcium carbonate powder is 90%-91%, and the percentage by weight of binding agent is 9%-10%.
As a preferred embodiment of the present invention, in described steps A, the median particle diameter of described calcium carbonate powder is 14-15 μm.
Further, in described steps A, described calcium carbonate powder distribution of particle sizes is:
D0.5：14-15μm；
D0.1：5.2-6.5μm；
D0.9：29-30.5μm；
D[4，3]：15.5-17.2μm。
Further, described steps A comprises the step choosing calcium carbonate powder granularity;
Choose the calcium carbonate powder of satisfied following distribution of particle sizes:
D0.5：14-15μm；
D0.1：5.2-6.5μm；
D0.9：29-30.5μm；
D[4，3]：15.5-17.2μm。
As a preferred embodiment of the present invention, the calcium carbonate powder in described steps A be the winnofil PCC that generated by fine natural magnesium calcium powder FGCC and high-purity chemical reaction method by a certain percentage Homogeneous phase mixing form; Fine natural magnesium calcium powder FGCC is processed through crushing and classification by food-class high-purity natural whiting GCC; The mixed weight ratio of FGCC and PCC is X: Y, wherein, and 20 < X < 100,0 < Y < 80.
As a preferred embodiment of the present invention, in described calcium carbonate powder, containing percetage by weight≤0.01% of manganese; Containing percetage by weight≤0.0002% of arsenic salt; Mercurous percetage by weight≤0.00003%; Leaded percetage by weight 0.0003%, containing the percetage by weight 0.002% of heavy metal.The mean diameter of described calcium carbonate powder is 4-30 μm, and bulk density is 0.4-1.7g/ml.
As a preferred embodiment of the present invention, in step B, temperature controls at 65 ± 2 DEG C.
As a preferred embodiment of the present invention, described high-density calcium carbonate particles bulk density exists: 0.80g/ml-1.40g/ml, and compactness exists: 0.95g/ml-1.60g/ml.
Beneficial effect of the present invention is: the high-density calcium carbonate particles manufactured by the manufacture method utilizing the present invention to propose, and its distribution of particle sizes is even, and granularity is relatively concentrated, the mobility of product is fine, be conducive at sheeting stages, sheet weight average is even, and compressibility is good.Can machine loss be reduced simultaneously, increase the service life.
Accompanying drawing explanation
Fig. 1 is the flow chart of manufacture method of the present invention.
Fig. 2 is the Malvern granularity graph of the Paris white powder stock that embodiment one adopts.
Fig. 3 is ordinary calcium carbonate Malvern granularity graph.
Detailed description of the invention
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
Embodiment one
High-density calcium carbonate particles, also can be described as Direct Compress Calcium Carbonate (vertical compression type calcium carbonate granule), is a kind ofly directly to make the raw material of calcium tablet by tabletting; The product such as now commercially available " calcium magnesium slice ", " compound vitamin calcium tablet ", chewable tablet all can with this high-density calcium carbonate particles as raw material.After system of the present invention uses calcium carbonate classified, wet granulation, granulate, drying, sieve, mix.
Refer to Fig. 1, present invention is disclosed a kind of manufacture method of high-density calcium carbonate particles, the method comprises the steps:
[steps A] chooses calcium carbonate powder granularity, is joined in mixer-granulator by calcium carbonate powder.
In the present embodiment, the raw material of calcium carbonate powder is high purity medical calcium carbonate, and this calcium carbonate, based on natural whiting, has that calcium carbonate content is high, impurity is few, that poisonous and harmful element is low is special, be beneficial to the absorption of human body, reduce the damage to human body.This raw material meets YBH0581 (2004) standard (as shown in table 1) obtaining the approval of national Bureau of Drugs Supervision.
Table 1
Obtain high-density calcium carbonate particles, the particle size distribution of high purity medical calcium carbonate is very important.Find through test of many times: to calcium carbonate scope as shown in Figure 2 just very applicable the present invention as calcium raw material; The Malvern particle size distribution figure of above-mentioned raw materials is shown in Fig. 2, and ordinary calcium carbonate Malvern granularity graph is shown in Fig. 3.
As can be seen from Figure 2, the particle size distribution of the purity calcium carbonate raw material that this patent uses is different from other common products, and granularity concentrates on 14.51 microns mostly, and the span scope of particle diameter is little, and concrete data are in table 2:
| Project | Numerical value (micron) |
| d 0.5 | 14-15 |
| d 0.1 | 5.2-6.5 |
| d 0.9 | 29-30.5 |
| D[4，3] | 15.5-17.2 |
Table 2
Binding agent and water are sized mixing by [step B], and temperature controls setting value (as 65 ± 2 DEG C, controlling at 66.5 DEG C in the present embodiment), the binding agent after sizing mixing and water are sprayed in mixer-granulator and granulate.In the present embodiment, binding agent is pregelatinized Starch.The percentage by weight of calcium carbonate powder is 90%-91%, and the percentage by weight of binding agent is 9%-10%.In the present embodiment, the percentage by weight of calcium carbonate powder is 90.98%, and the percentage by weight of binding agent is 9.02%.
The binding agent that general routine uses has CMC, PVPk30, maltodextrin, and the effect of these binding agents is pretty good, but expense is very expensive.
price be 280 yuan/price of kg, CMC is 50 yuan/kg, the price of maltodextrin is 25 yuan/kg.And the present invention uses pregelatinized Starch as binding agent, the price of pregelatinized Starch, well below the above two, only has 8 yuan/kg.And the product that the granular mass of pregelatinized Starch manufacture manufactures higher than the above two binding agents, therefore can reduce costs greatly.
Existing method of granulating is that one-step method is granulated, and is a kind of wet granulation.So-called one-step method is exactly first calcium carbonate and binding agent are directly added in granulator, then after water filling granulates, dry, screening, mixed processes.
And calcium carbonate first joins in mixer-granulator by the present invention; binding agent and water control under uniform temperature after sizing mixing; spray in mixer-granulator and granulate, the particle uniformity of working it out like this is good, and quality is better than the granule of external one-step method granulation gained greatly.
[step C] carries out pre-drying step before granulate, then granulate.
The conventional drying operation of wet granulation adopts a step dry.Find through test of many times, one-step method drying will be far superior to through the dried granular mass of two step method.Product of the present invention, first by predrying rear granulate, improves the uniformity of granule, reduces fine powder, good fluidity.And during external one-step method granulates, use be also a step seasoning, far away not as good as the calcium carbonate granule utilizing manufacture method of the present invention to produce in the uniformity, mobility of granule.
[step D] carries out dried to the granule after step C process;
[step e], by screening, is divided into granule the granule section varied in size;
[step F] blend step.
The present invention, compared with other like products, has following advantage:
High-density calcium carbonate particles of the present invention is as the primary raw material of calcium tablet, and its superiority is not only embodied in its chemistry and physical index, makes the advantage after calcium tablet in addition: the density 1) improving tablet; 2) production output is improved; 3) reduce machine loss, increase the service life.
The present invention is with regard to granule, and its distribution of particle sizes is even, and granularity is relatively concentrated, and the mobility of product is beneficial to very well like this at sheeting stages, and sheet weight average is even, and compressibility is good.
1, formulation selection
The formula of high-density calcium carbonate particles of the present invention, through test of many times, test is in table 3.
| Adjuvant percentage by weight | 5％ | 9.08％ | 12％ |
| 20 screen residues (%) | 6.5 | 3.5 | 0 |
| 200 screen residues (%) | 75 | 90 | 100％ |
| Conclusion | Fine powder is too much | Moderate | Partially thick and granule is harder |
Table 3
According to the sample that above-mentioned 3 proportionings are produced, carry out tabletting test, find:
1) granule of adjuvant percentage by weight 5%, because fine powder is too many during tabletting, slice, thin piece becomes type hardness tester undesirable ,≤200kn.
2) adjuvant percentage by weight 9.08%, uniform granularity, slice, thin piece molding, hardness is at about 250kn, and slice, thin piece fineness is good; Tableting pressure is little, and pressure is about about 3kn, reduces drift wearing and tearing.
3) adjuvant percentage by weight 12%, granule increases because of ratio of binder, and granule is harder.In the granulate stage, particle is really up to the mark, when tabletting, tableting pressure substantially at 6-7kn, drift serious wear.
According to above-mentioned experiment, select calcium carbonate weight percent 90.98%, the proportioning superiority of adjuvant (pregelatinized Starch) percentage by weight 9.08% is obvious.
2, mobility contrast
The mobility of high-density calcium carbonate particles of the present invention is better than general granule, and to carry out testing the result compared as follows with other granules.
Test specific as follows:
1) testing equipment: Powerer Flowability Index Test Instrument (powder flowbility index test instrument)
2) subjects: product of the present invention, conventional granulates
3) test procedure:
A, first weigh a certain amount of granule.
B, by product of the present invention and conventional granulates successively by aperture, see mobility.
C, granule pass through completely, see the aperture of screen cloth.
According to this test procedure, test data is as table 4:
| Product | Conventional granulates | Product of the present invention |
| Mobility | 6mm | 4mm |
Table 4
The liquidity scale carrys out the mobility quality of constant product with the size in aperture.Aperture is less, and mobility is better; Otherwise mobility is then poorer.
3, volume vs
The scope of the degree of tightness density domination of high-density calcium carbonate particles of the present invention is very tight:
Bulk density exists: 0.80g/ml-1.40g/ml, and compactness exists: 0.95g/ml-1.60g/ml.Such standard is very crucial for later stage result of use of the present invention.
Utilize the calcium tablet that high-density calcium carbonate particles of the present invention is suppressed, compare with like product on market, and with " calcium carbonate D
3sheet " in the identical situation of formula in average sheet at about 1.8g, volume is 0.9ml, and density is 2g/ml.Its compression performance is good, and comparatively " calcium carbonate D3 sheet ", volume reduces 15%; Comparatively " calcium carbonate chewable tablet ", volume reduces 30%; Concrete data are in table 5.
Wherein, calcium content and " the calcium carbonate D of high density calcium tablet of the present invention
3sheet " identical, be 600mg/ sheet, and the calcium content of " calcium carbonate chewable tablet " is 500mg/ sheet.
| Title | Calcium carbonate D 3Sheet | Calcium carbonate chewable tablet | The present invention |
| The heavy g of sheet | 1.8 | 2.5 | 1.8 |
| Volume ml | 1 | 1.5 | 0.9 |
| Density g/ml | 1.8 | 1.67 | 2 |
| Calcium content mg/ sheet | 600 | 500 | 600 |
Table 5
4, disintegration compares
For tablet, disintegration is a very important index.Because tablet reaches stomach, need short time complete disintegrate, so disintegration is self-evident for the importance of tablet.
High-density calcium carbonate particles of the present invention according to " calcium carbonate D
3sheet " the obtained tablet of same recipe tabletting, carries out test and comparison disintegration.
Test specific as follows:
1) testing equipment: LB-2D intelligence disintegration time tester (Shanghai Huanghai Sea medicine inspection Instrument Ltd.)
2) subjects: product of the present invention, " calcium carbonate D
3sheet "
3) test procedure:
A, first instrument is carried out preheating, water temperature controls 37 DEG C ± 1 DEG C.
B, by product of the present invention 6 and " calcium carbonate D
3sheet " 6 slices, drop into respectively in 2 hanging baskets.
C, by start key, hanging basket moves up and down, and tablet is in disintegrate slowly.
After D, 6 tablets of tablets dissolve all completely, writing time.
According to this test procedure, test data is as shown in table 6:
| Product | Calcium carbonate D 3Sheet | Product of the present invention |
| Disintegration time | 3″ | 2″30′ |
Table 6
5, machine loss reduces
The hardness of tablet is also the index of an outbalance.If tablet hardness is inadequate, is easy to fracture, and affects attractive in appearance.And in the technique of producing, it is a technical barrier that the tableting pressure as how less reaches satisfied hardness.
For sheeting equipment, pressure used is less, and the loss for equipment is less, like this can service time of extension device.
High-density calcium carbonate particles of the present invention just in time solves this difficult problem.Because uniform particles, compressibility is good, reaching under identical hardness, can reduce tableting pressure.
The common calcium carbonate granule of general use carries out tabletting, and tableting pressure is when 5-6kn, and the hardness of tablet can reach 200kn; And high-compressibility calcium carbonate granule of the present invention, tableting pressure is at about 3kn, and the hardness of tablet can reach 250kn.Pressure drop nearly 50%.During such production, the damage of mechanical wear and drift can be reduced, extension device service life.Directly have influence on the sunk cost of product the service life of drift, during tabletting, pressure is less, and drift wearing and tearing are fewer, and service life is longer, and sunk cost is lower.
In sum, the high-density calcium carbonate particles manufactured by the manufacture method utilizing the present invention to propose, its distribution of particle sizes is even, and granularity is relatively concentrated, and the mobility of product is fine, and be conducive at sheeting stages, sheet weight average is even, and compressibility is good; Can machine loss be reduced simultaneously, increase the service life.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments.Distortion and the change of embodiment disclosed are here possible, are known for the replacement of embodiment those those of ordinary skill in the art and the various parts of equivalence.Those skilled in the art are noted that when not departing from spirit of the present invention or substitutive characteristics, the present invention can in other forms, structure, layout, ratio, and to realize with other assembly, material and parts.When not departing from the scope of the invention and spirit, can other distortion be carried out here to disclosed embodiment and change.
Claims (8)
1. a manufacture method for high-density calcium carbonate particles, is characterized in that, the method comprises the steps:
A, calcium carbonate powder is joined in mixer-granulator;
B, binding agent and water are sized mixing, temperature controls in setting value, the binding agent after sizing mixing and water is sprayed in mixer-granulator and granulates;
C, granulate step;
D, dried is carried out to the granule after step C process;
E, by screening, granule is divided into the granule section varied in size;
F, blend step;
In described steps A, the median particle diameter of described calcium carbonate powder is 14-15 μm;
Described steps A comprises the step choosing calcium carbonate powder granularity;
Choose the calcium carbonate powder of satisfied following distribution of particle sizes:
D0.5：14-15μm；
D0.1：5.2-6.5μm；
D0.9：29-30.5μm；
D[4,3]：15.5-17.2μm。
2. the manufacture method of high-density calcium carbonate particles according to claim 1, is characterized in that:
In described step C, before granulate, carry out pre-drying step, then granulate.
3. the manufacture method of high-density calcium carbonate particles according to claim 1, is characterized in that:
Binding agent in described step B is pregelatinized Starch.
4., according to the manufacture method of the high-density calcium carbonate particles one of claims 1 to 3 Suo Shu, it is characterized in that:
The percentage by weight of calcium carbonate powder is 90%-91%,
The percentage by weight of binding agent is 9%-10%.
5. the manufacture method of high-density calcium carbonate particles according to claim 1, is characterized in that:
Calcium carbonate powder in described steps A be the winnofil PCC that generated by fine natural magnesium calcium powder FGCC and high-purity chemical reaction method by a certain percentage Homogeneous phase mixing form;
Fine natural magnesium calcium powder FGCC is processed through crushing and classification by food-class high-purity natural whiting GCC;
The mixed weight ratio of FGCC and PCC is X:Y, wherein, and 20<X<100,0<Y<80.
6., according to the manufacture method of the high-density calcium carbonate particles one of claim 1 to 5 Suo Shu, it is characterized in that:
In described calcium carbonate powder, the Chong containing manganese measures Bai Fen Shuo≤0.01%; Chong containing arsenic salt measures Bai Fen Shuo≤0.0002%; Mercurous Chong measures Bai Fen Shuo≤0.00003%; Leaded percetage by weight 0.0003%, containing the percetage by weight 0.002% of heavy metal; The mean diameter of described calcium carbonate powder is 4-30 μm, and bulk density is 0.4-1.7g/ml.
7., according to the manufacture method of the high-density calcium carbonate particles one of claim 1 to 5 Suo Shu, it is characterized in that:
In step B, temperature controls at 65 ± 2 DEG C.
8., according to the manufacture method of the high-density calcium carbonate particles one of claim 1 to 5 Suo Shu, it is characterized in that:
Described high-density calcium carbonate particles bulk density exists: 0.80g/ml-1.40g/ml, and compactness exists: 0.95g/ml-1.60g/ml.
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| CN103565826A (en) * | 2013-10-16 | 2014-02-12 | 池州市大恒生化有限公司 | High-density compound calcium carbonate |
| CN106389344A (en) * | 2016-10-18 | 2017-02-15 | 广州中大南沙科技创新产业园有限公司 | Calcium carbonate particles and preparation method thereof |
| CN112972402B (en) * | 2021-03-26 | 2022-09-20 | 那生桑 | Oil-containing Mongolian medicine powder formula granule and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1189458A (en) * | 1996-12-27 | 1998-08-05 | 奥多摩工业株式会社 | Aqueous slurry of precipitated calcium carbonate and ground calcium carbonate in combination |
| CN1326338A (en) * | 1998-11-13 | 2001-12-12 | 尼康姆德法尔马公司 | Process for preparing oral calcium compositions |
| CN1860351A (en) * | 2003-07-31 | 2006-11-08 | 德拉沃有限责任公司 | Calcium carbonate granulation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1189458A (en) * | 1996-12-27 | 1998-08-05 | 奥多摩工业株式会社 | Aqueous slurry of precipitated calcium carbonate and ground calcium carbonate in combination |
| CN1326338A (en) * | 1998-11-13 | 2001-12-12 | 尼康姆德法尔马公司 | Process for preparing oral calcium compositions |
| CN1860351A (en) * | 2003-07-31 | 2006-11-08 | 德拉沃有限责任公司 | Calcium carbonate granulation |
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