CN102106870A - Method for preparing high-density calcium carbonate granules - Google Patents
Method for preparing high-density calcium carbonate granules Download PDFInfo
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- CN102106870A CN102106870A CN2009101993449A CN200910199344A CN102106870A CN 102106870 A CN102106870 A CN 102106870A CN 2009101993449 A CN2009101993449 A CN 2009101993449A CN 200910199344 A CN200910199344 A CN 200910199344A CN 102106870 A CN102106870 A CN 102106870A
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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 the inorganic chemicals industry technical field, relate to a kind of high density carbonic acid calcium granule, relate in particular to the particulate manufacture method of a kind of high density carbonic acid calcium.
Background technology
Calcium is the maximum metallic element of people's in-vivo content, and 1200 grams are arranged approximately, also is one of element of the easiest shortage.Wherein 99% be formed at skeleton, 1% is present in the blood soft tissue.Whether calcium deficiency is relevant with two aspect reasons for human body: the one, and the peak bone amount, promptly when one's mid-30s, the calcium content when human body bone amount reaches in life high bone mass is mainly by inherited genetic factors, the factor of replenishing the calcium and exercise factors decision; The 2nd, the calcium loss situation is determined by the replenishing of calcium, number of dropouts and living habit, as it is too high to have a liking for tobacco and wine, coffee, tea, cola, salt intake, eats meat less or eats the loss that too many meat all can cause calcium.
The general calcium carbonate that adopts from natural origin of edible calsium supplement comprises limestone and Concha Ostreae.Recommend according to Chinese Soclety of Nutrition, the magnitude of recruitment of one day calcium of adult is at 600mg.Therefore, the instructions of taking that replenishes calcium preparation is taken the calcium tablet that a slice contains 600mg calcium general every day.Even but like this, most of calcium tablets are still very big, dysphagia or make us uncomfortable.Therefore, some occur and reduced 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: provide a kind of high density carbonic acid calcium particulate manufacture method, can effectively improve the density of tablet.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
The particulate manufacture method of a kind of high density carbonic acid calcium, this method comprises the steps:
A, calcium carbonate powder is joined in the mixer-granulator;
B, binding agent and water are sized mixing, temperature is controlled under the setting value, the binding agent after sizing mixing and water is sprayed in the mixer-granulator granulate;
C, granulate step;
D, the granule after handling through step C is carried out dried;
E, by the screening, granule is divided into the granule section that varies in size;
F, blend step.
As a preferred embodiment of the present invention, among the described step C, before granulate, carry out predrying step, then granulate.
As a preferred embodiment of the present invention, the binding agent among the 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 the described steps A, the median particle diameter of described calcium carbonate powder is 14-15 μ m.
Further, in the 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, comprise the step of choosing the calcium carbonate powder granularity in the described steps A;
Choose the calcium carbonate powder that satisfies 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 the described steps A be the winnofil PCC that generates by fine natural magnesium calcium powder FGCC and high-purity chemical reaction method by a certain percentage uniform 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 the described calcium carbonate powder, manganiferous percetage by weight≤0.01%; Percetage by weight≤0.0002% that contains arsenic salt; Mercurous percetage by weight≤0.00003%; Plumbiferous percetage by weight 0.0003% contains the percetage by weight 0.002% of heavy metal.The mean diameter of described calcium carbonate powder is 4-30 μ m, and bulk density is 0.4-1.7g/ml.
As a preferred embodiment of the present invention, among the step B, temperature is controlled at 65 ± 2 ℃.
As a preferred embodiment of the present invention, described high density carbonic acid calcium granule bulk density exists: 0.80g/ml-1.40g/ml, compactness exists: 0.95g/ml-1.60g/ml.
Beneficial effect of the present invention is: utilize the high density carbonic acid calcium granule of the manufacture method manufacturing that the present invention proposes, its distribution of particle sizes is even, and granularity is relatively concentrated, product mobile fine, help in the tabletting stage, the sheet weight average is even, and compressibility is good.Simultaneously can reduce machine loss, increase the service life.
Description of drawings
Fig. 1 is the flow chart of manufacture method of the present invention.
Fig. 2 is the Ma Erwen granularity graph of the Paris white powder stock of embodiment one employing.
Fig. 3 is an ordinary calcium carbonate Ma Erwen granularity graph.
The specific embodiment
Describe the preferred embodiments of the present invention in detail below in conjunction with accompanying drawing.
Embodiment one
High density carbonic acid calcium granule also can be described as Direct Compress Calcium Carbonate (vertical compression type calcium carbonate granule), is a kind of raw material of directly can tabletting making calcium tablet; All available these high density carbonic acid calcium granules of product such as now commercially available " calcium magnesium slice ", " compound vitamin calcium tablet ", chewable tablet are as raw material.The present invention is after using calcium carbonate classified, wet granulation, granulate, drying, sieves, mixes.
See also Fig. 1, the present invention has disclosed the particulate manufacture method of a kind of high density carbonic acid calcium, and this method comprises the steps:
[steps A] chooses the calcium carbonate powder granularity, and calcium carbonate powder is joined in the mixer-granulator.
In the present embodiment, the raw material of calcium carbonate powder is the high purity medical calcium carbonate, and this calcium carbonate is based on natural whiting, has the calcium carbonate content height, that impurity is few, poisonous and harmful element is low is special, is beneficial to absorption by human body, reduces the damage to human body.This raw material meets YBH0581 (2004) standard (as shown in table 1) that obtains the approval of national Bureau of Drugs Supervision.
Table 1
Make high density carbonic acid calcium granule, the particle size distribution of high purity medical calcium carbonate is very important.Find through test of many times: to calcium carbonate in just very suitable the present invention of scope as shown in Figure 2 as the calcium raw material; The Ma Erwen particle size distribution figure of above-mentioned raw materials is seen Fig. 2, and ordinary calcium carbonate Ma Erwen granularity graph is seen Fig. 3.
As can be seen from Figure 2, the particle size distribution of the employed purity calcium carbonate raw material of this patent is different with other common products, and granularity concentrates on about 14.51 microns mostly, and the span scope of particle diameter is little, and concrete data see 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
[step B] sizes mixing binding agent and water, and temperature is controlled at setting value (as 65 ± 2 ℃, being controlled at 66.5 ℃ in the present embodiment), the binding agent after sizing mixing and water sprayed in the mixer-granulator 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 general conventional binding agent that uses has CMC, PVPk30, maltodextrin, and the effect of these binding agents is pretty good, but expense is very expensive.
Price be 280 yuan/kg, the price of CMC is 50 yuan/kg, the price of maltodextrin is 25 yuan/kg.And the present invention uses pregelatinized Starch as binding agent, and the price of pregelatinized Starch has only 8 yuan/kg well below the above two.And the granular mass of pregelatinized Starch manufacturing is higher than the product that the above two binding agents are made, and therefore can reduce cost greatly.
Existing method of granulating is that one-step method is granulated, and is a kind of wet granulation.So-called one-step method directly adds calcium carbonate and binding agent in the granulator earlier exactly, after water filling is granulated again, and drying, screening, mixed processes.
And the present invention joins calcium carbonate in the mixer-granulator earlier; after sizing mixing, binding agent and water is controlled under the uniform temperature; spray in the mixer-granulator and granulate, the uniform particles 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 predrying step, then granulate before granulate.
The conventional drying operation of wet granulation adopts a step dry.Find through test of many times, will be far superior to the one-step method drying through the dried granular mass of two step method.Product of the present invention by predrying back granulate, improves the particulate uniformity earlier, reduces fine powder, good fluidity.And during external one-step method granulates, use also be a step seasoning, on particulate uniformity, flowability far away not as good as the calcium carbonate granule that utilizes manufacture method of the present invention to produce.
[step D] carries out dried to the granule after handling through step C;
[step e] is divided into granule the granule section that varies in size by screening;
[step F] blend step.
The present invention compares with other like products, and following advantage is arranged:
High density carbonic acid calcium granule of the present invention is as the primary raw material of calcium tablet, and its superiority not only is embodied on its chemistry and the physical index, makes the advantage behind the calcium tablet in addition: the density that 1) improves tablet; 2) improve production output; 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 mobile fine of product was beneficial to like this in the tabletting stage, and the sheet weight average is even, and compressibility is good.
1, formulation selection
The particulate prescription of high density carbonic acid calcium of the present invention, through test of many times, test sees Table 3.
| The 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 | Thick partially and granule is harder |
Table 3
According to the sample that above-mentioned 3 proportionings are produced, carry out the tabletting test, find:
1) granule of adjuvant percentage by weight 5%, because fine powder is too many, slice, thin piece becomes type hardness tester undesirable ,≤200kn during tabletting.
2) the adjuvant percentage by weight 9.08%, uniform granularity, and the slice, thin piece molding, hardness is about 250kn, and slice, thin piece fineness is good; Tabletting pressure is little, about the about 3kn of pressure, reduces the drift wearing and tearing.
3) the adjuvant percentage by weight 12%, and granule increases because of the binding agent adding proportion, and granule is harder.In the granulate stage, particle is really up to the mark, and when tabletting, tabletting pressure is substantially at 6-7kn, the drift serious wear.
According to above-mentioned experiment, select weight of calcium carbonate percentage ratio 90.98%, the proportioning superiority of adjuvant (pregelatinized Starch) percentage by weight 9.08% is obvious.
2, mobile contrast
The particulate flowability of high density carbonic acid calcium of the present invention is better than general granule, and the result who tests comparison with other granules is as follows.
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, a certain amount of granule of first weighing.
B, with product of the present invention and conventional granulates successively by the aperture, see flowability.
C, granule pass through fully, see the aperture of screen cloth.
According to this test procedure, test data such as table 4:
| Product | Conventional granulates | Product of the present invention |
| Mobile | 6mm | 4mm |
Table 4
The liquidity scale comes the mobile quality of constant product with the size in aperture.The aperture is more little, and flowability is good more; Otherwise flowability is then poor more.
3, volume contrast
The scope of the particulate degree of tightness density control of high density carbonic acid calcium of the present invention is very tight:
Bulk density exists: 0.80g/ml-1.40g/ml, 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 of high density carbonic acid calcium granule of the present invention compacting, compare with like product on the market, and with " calcium carbonate D
3Sheet " under the identical situation of prescription in the average sheet about 1.8g, volume is 0.9ml, density is 2g/ml.Its compression performance is good, and " calcium carbonate D3 sheet ", volume reduces 15%; " calcium carbonate chewable tablet ", volume reduces 30%; Concrete data see Table 5.
Wherein, the calcium content of high density calcium tablet of the present invention and " calcium carbonate D
3Sheet " identical, be the 600mg/ sheet, and the calcium content of " calcium carbonate chewable tablet " is the 500mg/ sheet.
| Title | Calcium carbonate D 3Sheet | The calcium carbonate chewable tablet | The present invention |
| The heavy g of sheet | 1.8 | 2.5 | 1.8 |
| |
1 | 1.5 | 0.9 |
| Density g/ml | 1.8 | 1.67 | 2 |
| Calcium content mg/ sheet | 600 | 500 | 600 |
Table 5
4, disintegration relatively
For tablet, disintegration is a crucial index.Because tablet reaches stomach, need complete disintegrate of short time, so disintegration is self-evident for the importance of tablet.
High density carbonic acid calcium granule basis of the present invention and " calcium carbonate D
3Sheet " tablet that makes of same recipe tabletting, carry out test disintegration relatively.
Test specific as follows:
1) testing equipment: LB-2D intelligence instrument disintegration (Shanghai Huanghai Sea medicine inspection Instr Ltd.)
2) subjects: product of the present invention, " calcium carbonate D
3Sheet "
3) test procedure:
A, elder generation carry out preheating with instrument, 37 ℃ ± 1 ℃ of water temperature control.
B, with 6 of products of the present invention and " calcium carbonate D
3Sheet " 6 slices, drop into respectively in 2 hanging baskets.
C, press start key, hanging basket moves up and down, and tablet is in disintegrate slowly.
After D, 6 tablets of tablets dissolve all fully, 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 also is the index of an outbalance.If tablet hardness is not enough, is easy to fracture, and influences attractive in appearance.And on the technology of producing, reaching satisfied hardness as how less tabletting pressure is a technical barrier.
For sheeting equipment, used pressure is more little, and is just more little for the loss of equipment, can prolong the service time of equipment like this.
High density carbonic acid calcium granule of the present invention has just in time solved this difficult problem.Because uniform particles, compressibility is good, reaching under the identical hardness, can reduce tabletting pressure.
The common calcium carbonate granule of general use carries out tabletting, and tabletting pressure is in 5-6kn, and the hardness of tablet can reach 200kn; And high-compressibility calcium carbonate granule of the present invention, tabletting pressure is about 3kn, and the hardness of tablet can reach 250kn.Pressure has nearly descended 50%.When producing like this, can reduce the damage of mechanical wear and drift, prolong service life of equipment.Directly have influence on the sunk cost of product the service life of drift, and pressure is more little during tabletting, and the drift wearing and tearing are few more, and service life is long more, and sunk cost is low more.
In sum, utilize the high density carbonic acid calcium granule of the manufacture method manufacturing that the present invention proposes, its distribution of particle sizes is even, and granularity is relatively concentrated, and product mobile fine helped in the tabletting stage, and the sheet weight average is even, and compressibility is good; Simultaneously can reduce machine loss, increase the service life.
Here description of the invention and application is illustrative, is not to want with scope restriction of the present invention in the above-described embodiments.Here the distortion of disclosed embodiment and change are possible, and the various parts of the replacement of embodiment and equivalence are known for those those of ordinary skill in the art.Those skilled in the art are noted that under the situation that does not break away from spirit of the present invention or substitutive characteristics, and the present invention can be with other form, structure, layout, ratio, and realize with other assembly, material and parts.Under the situation that does not break away from the scope of the invention and spirit, can carry out other distortion and change here to disclosed embodiment.
Claims (10)
1. the particulate manufacture method of high density carbonic acid calcium is characterized in that this method comprises the steps:
A, calcium carbonate powder is joined in the mixer-granulator;
B, binding agent and water are sized mixing, temperature is controlled at setting value, the binding agent after sizing mixing and water is sprayed in the mixer-granulator granulate;
C, granulate step;
D, the granule after handling through step C is carried out dried;
E, by the screening, granule is divided into the granule section that varies in size;
F, blend step.
2. the particulate manufacture method of high density carbonic acid calcium according to claim 1 is characterized in that:
Among the described step C, before granulate, carry out predrying step, then granulate.
3. the particulate manufacture method of high density carbonic acid calcium according to claim 1 is characterized in that:
Binding agent among the described step B is pregelatinized Starch.
4. according to the particulate manufacture method of the described high density carbonic acid of one of claim 1 to 3 calcium, 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 particulate manufacture method of high density carbonic acid calcium according to claim 1 is characterized in that:
In the described steps A, the median particle diameter of described calcium carbonate powder is 14-15 μ m.
6. the particulate manufacture method of high density carbonic acid calcium according to claim 5 is characterized in that:
Comprise the step of choosing the calcium carbonate powder granularity in the described steps A;
Choose the calcium carbonate powder that satisfies 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。
7. the particulate manufacture method of high density carbonic acid calcium according to claim 1 is characterized in that:
Calcium carbonate powder in the described steps A be the winnofil PCC that generates by fine natural magnesium calcium powder FGCC and high-purity chemical reaction method by a certain percentage uniform 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.
8. according to the particulate manufacture method of the described high density carbonic acid of one of claim 1 to 7 calcium, it is characterized in that:
In the described calcium carbonate powder, manganiferous percetage by weight≤0.01%; Percetage by weight≤0.0002% that contains arsenic salt; Mercurous percetage by weight≤0.00003%; Plumbiferous percetage by weight 0.0003% contains the percetage by weight 0.002% of heavy metal; The mean diameter of described calcium carbonate powder is 4-30 μ m, and bulk density is 0.4-1.7g/ml.
9. according to the particulate manufacture method of the described high density carbonic acid of one of claim 1 to 7 calcium, it is characterized in that:
Among the step B, temperature is controlled at 65 ± 2 ℃.
10. according to the particulate manufacture method of the described high density carbonic acid of one of claim 1 to 7 calcium, it is characterized in that:
Described high density carbonic acid calcium granule bulk density exists: 0.80g/ml-1.40g/ml, compactness exists: 0.95g/ml-1.60g/ml.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112972402A (en) * | 2021-03-26 | 2021-06-18 | 宋宏春 | Oil-containing Mongolian medicine powder formula granule and preparation method thereof |
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| 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 |
-
2009
- 2009-11-25 CN CN200910199344.9A patent/CN102106870B/en active Active
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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112972402A (en) * | 2021-03-26 | 2021-06-18 | 宋宏春 | Oil-containing Mongolian medicine powder formula granule 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 |
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