CN105366702A - Production method of pharmaceutical-grade calcium carbonate - Google Patents
Production method of pharmaceutical-grade calcium carbonate Download PDFInfo
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- CN105366702A CN105366702A CN201510895381.9A CN201510895381A CN105366702A CN 105366702 A CN105366702 A CN 105366702A CN 201510895381 A CN201510895381 A CN 201510895381A CN 105366702 A CN105366702 A CN 105366702A
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Abstract
The invention discloses a production method of pharmaceutical-grade calcium carbonate. The production method comprises steps of smashing, homogenizing, grinding, modifying, and freeze drying. According to the production method, sodium carbonate and dodecyl dimethyl benzyl ammonium chloride are added in the step of homogenizing so as to increase subsequent grinding efficiency, and shorten grinding time; a water injector is arranged in an adopted grinding miller, sprayed atomized water is capable of increasing powder weight, and suspension of powder is not easily caused, so that a millstone material bed is stabilized, and it is beneficial for grinding via combined action with added sodium carbonate and dodecyl dimethyl benzyl ammonium chloride; the production method is high in pharmaceutical-grade calcium carbonate yield; purity of obtained pharmaceutical-grade calcium carbonate is high, and particle size distribution is uniform; energy cost in production process is low, at the same time aggregation of fine powder in a slurry in wet grinding is not caused; operation of the production method is simple; production is convenient; cost is low; and the production method is suitable for industrialized large-scale production.
Description
Technical field
The present invention relates to Inorganic nonmetal mineral Material Field, be specifically related to a kind of production method of medicinal calcium carbonate.
Background technology
Water-ground limestone, also known as grinding calcium carbonate, is with natural calcite, marble, chalk etc. for raw material, through mechanical disintegration, grinds the powder product reaching certain fineness.Be commonly referred to as fine ground calcium carbonate (FGCC) in the world.In order to district is than precipitated chalk in paper industry, proportion by subtraction GCC and PCC is called for short.Generally the product of median size below 12 μm is called heavy fine calcium carbonate, to distinguish general water-ground limestone.By purposes, calcium carbonate product is divided into that the special calcium of hilllock stone, the special calcium of seal gum, the special calcium of rubber, the special calcium of papermaking, the special calcium of plastics, the special calcium of paint, the special calcium of toothpaste, medical special calcium, fodder additives are special, food is special etc.Medicinal calcium carbonate is widely used in tablet of replenishing the calcium, and makes high-density calcium tablet and chewable tablet; Also can be used as tablet filler, thus increase the nutritive ingredient etc. in Stresstabs; After medicinal calcium carbonate granulation, calsium supplement punching of being more convenient for is shaped.Granular calcium carbonate, the direct compression being mainly used in calsium supplement is shaped, and be otherwise known as calcium carbonate D.C.; In addition, among the plastics that also can be used for toy for children and coating, can guarantee to meet FDA toy international standard.The main content of calcium carbonate is high, foreign matter content is low, and Pb, As, Hg, Fe equal size is extremely low.Some index meets and exceeds the requirement of American Pharmacopeia (USP28/31), European Pharmacopoeia (EP2002), British Pharmacopoeia (BP2002) and Chinese Pharmacopoeia (CP2005).
The production method of water-ground limestone mainly contains dry method and wet method two kinds of methods, and dry production efficiency is high, but the fineness of product is subject to the restriction of grinding and classification technique, is difficult to the coarse whiting product producing ultra-fine fineness.Wet production powder product fineness is higher, in grinding, modification can also be carried out out to powder, therefore adopt wet method to be commonly used to produce ultrafine heavy calcium product, but in wet production, relate to the operation such as configuration, grinding, drying of slurry, therefore production efficiency is lower, and energy consumption is also higher.But it is because medicinal calcium carbonate is due to the singularity of its purposes, therefore higher to the requirement of production technique.And there is the shortcomings such as productive rate is low, purity is not high, size distribution is uneven in the medical calcium carbonate that prior art is produced, and there is high, simultaneously in slurry the fine powder of energy consumption in process of production and also easily assemble in wet grinding, affect mill efficiency and quality product.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of production method of medicinal calcium carbonate is provided.
Object of the present invention is achieved through the following technical solutions: a kind of production method of medicinal calcium carbonate, and it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 20 ~ 40min, the rotating speed of stirrer is 800 ~ 1200r/min;
S3. grind: the marble after homogeneous is added in vertical mill and grinds, waterworks is provided with in vertical mill, atomized water spraying in the process of grinding, obtain powder, wherein, described vertical mill grinding temperature is 40 ~ 50 DEG C, grinding pressure is 8 ~ 12MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent in powder and stir, the temperature of stirring is 30 ~ 50 DEG C, and churning time is 30 ~ 45min, obtains wet stock;
S5. lyophilize: by wet stock-10 ~-25 DEG C, vacuum tightness be the environment of 1.5 ~ 5Pa under lyophilize, obtain medicinal calcium carbonate.
Further, the weight ratio of marble described in step S2, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 80 ~ 110:1 ~ 5:1;
Further, the granular size of powder described in step S3 is 1250 ~ 2500 orders.
Further, the weight ratio of powder described in step S4, properties-correcting agent and dispersion agent is 100:0.8 ~ 1.2:0.1 ~ 0.15.
Further, described dispersion agent is trolamine.
Further, described properties-correcting agent is any one in stearic acid, titanic acid ester or phosphoric acid ester.
The present invention has the following advantages:
1. the present invention adds sodium carbonate, dodecyl benzyl dimethyl ammonium chloride at homogenizing step, improves the efficiency of later stage grinding, reduces the time of grinding; And waterworks is provided with in shredder, the atomized water of ejection not only increases the own wt of powder, powder not easily by suspension get up to make the mill bed of material to stablize, and with the sodium carbonate added, dodecyl benzyl dimethyl ammonium chloride acting in conjunction, utilize grinding;
2. the medical calcium carbonate productive rate prepared of the inventive method is high, purity is high, even particle size distribution, and low, simultaneously in slurry the fine powder of energy consumption is not assembled in wet grinding in process of production;
3. present invention process is simple to operate, easy to prepare, cost is low, be applicable to industrialization scale operation.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated.
embodiment 1:a production method for medicinal calcium carbonate, it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 20min, the rotating speed of stirrer is 800r/min; The weight ratio of described marble, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 80:1:1;
S3. grind: added in vertical mill by the marble after homogeneous and grind, be provided with waterworks in vertical mill, atomized water spraying in the process of grinding, obtain powder, the granular size of described powder is 1250 orders; Wherein, described vertical mill grinding temperature is 40 DEG C, grinding pressure is 8MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent trolamine in powder and stir, the temperature of stirring is 30 DEG C, and churning time is 30min, obtains wet stock; The weight ratio of described powder, properties-correcting agent and dispersion agent is 100:0.8:0.1; Described properties-correcting agent is stearic acid;
S5. lyophilize: by wet stock-10 DEG C, vacuum tightness be the environment of 1.5Pa under lyophilize, obtain medicinal calcium carbonate.
embodiment 2:a production method for medicinal calcium carbonate, it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 40min, the rotating speed of stirrer is 1200r/min; The weight ratio of described marble, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 110:5:1;
S3. grind: added in vertical mill by the marble after homogeneous and grind, be provided with waterworks in vertical mill, atomized water spraying in the process of grinding, obtain powder, the granular size of described powder is 2500 orders; Wherein, described vertical mill grinding temperature is 50 DEG C, grinding pressure is 12MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent trolamine in powder and stir, the temperature of stirring is 50 DEG C, and churning time is 45min, obtains wet stock; The weight ratio of described powder, properties-correcting agent and dispersion agent is 100:1.2:0.15; Described properties-correcting agent is titanic acid ester;
S5. lyophilize: by wet stock-25 DEG C, vacuum tightness be the environment of 5Pa under lyophilize, obtain medicinal calcium carbonate.
embodiment 3:a production method for medicinal calcium carbonate, it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 28min, the rotating speed of stirrer is 1000r/min; The weight ratio of described marble, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 90:2:1;
S3. grind: added in vertical mill by the marble after homogeneous and grind, be provided with waterworks in vertical mill, atomized water spraying in the process of grinding, obtain powder, the granular size of described powder is 2000 orders; Wherein, described vertical mill grinding temperature is 42 DEG C, grinding pressure is 9MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent trolamine in powder and stir, the temperature of stirring is 38 DEG C, and churning time is 35min, obtains wet stock; The weight ratio of described powder, properties-correcting agent and dispersion agent is 100:0.9:0.12; Described properties-correcting agent is phosphoric acid ester;
S5. lyophilize: by wet stock-15 DEG C, vacuum tightness be the environment of 2.8Pa under lyophilize, obtain medicinal calcium carbonate.
embodiment 4:a production method for medicinal calcium carbonate, it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 35min, the rotating speed of stirrer is 1150r/min; The weight ratio of described marble, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 105:4.5:1;
S3. grind: added in vertical mill by the marble after homogeneous and grind, be provided with waterworks in vertical mill, atomized water spraying in the process of grinding, obtain powder, the granular size of described powder is 2500 orders; Wherein, described vertical mill grinding temperature is 48 DEG C, grinding pressure is 11MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent trolamine in powder and stir, the temperature of stirring is 45 DEG C, and churning time is 42min, obtains wet stock; The weight ratio of described powder, properties-correcting agent and dispersion agent is 100:1.1:0.13; Described properties-correcting agent is stearic acid;
S5. lyophilize: by wet stock-20 DEG C, vacuum tightness be the environment of 4Pa under lyophilize, obtain medicinal calcium carbonate.
Claims (6)
1. a production method for medicinal calcium carbonate, is characterized in that, it comprises the following steps:
S1. broken: marble to be used high pressure water washing stone, to remove after the earth of block faces and dust by crusher in crushing to grain diameter≤40mm;
S2. homogeneous: add sodium carbonate in the marble pulverized, dodecyl benzyl dimethyl ammonium chloride stirs 20 ~ 40min, the rotating speed of stirrer is 800 ~ 1200r/min;
S3. grind: the marble after homogeneous is added in vertical mill and grinds, waterworks is provided with in vertical mill, atomized water spraying in the process of grinding, obtain powder, wherein, described vertical mill grinding temperature is 40 ~ 50 DEG C, grinding pressure is 8 ~ 12MPa, moisture controlled index≤0.3% of described powder;
S4. modification: add water, properties-correcting agent and dispersion agent in powder and stir, the temperature of stirring is 30 ~ 50 DEG C, and churning time is 30 ~ 45min, obtains wet stock;
S5. lyophilize: by wet stock-10 ~-25 DEG C, vacuum tightness be the environment of 1.5 ~ 5Pa under lyophilize, obtain medicinal calcium carbonate.
2. the preparation method of a kind of medicinal calcium carbonate as claimed in claim 1, is characterized in that, the weight ratio of marble described in step S2, sodium carbonate and dodecyl benzyl dimethyl ammonium chloride is 80 ~ 110:1 ~ 5:1.
3. the preparation method of a kind of medicinal calcium carbonate as claimed in claim 1, is characterized in that, the granular size of powder described in step S3 is 1250 ~ 2500 orders.
4. the preparation method of a kind of medicinal calcium carbonate as claimed in claim 1, is characterized in that, the weight ratio of powder described in step S4, properties-correcting agent and dispersion agent is 100:0.8 ~ 1.2:0.1 ~ 0.15.
5. the preparation method of a kind of medicinal calcium carbonate as described in claim 1 or 4, is characterized in that, described dispersion agent is trolamine.
6. the preparation method of a kind of medicinal calcium carbonate as described in claim 1 or 4, is characterized in that, described properties-correcting agent is any one in stearic acid, titanic acid ester or phosphoric acid ester.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163595A (en) * | 2017-05-31 | 2017-09-15 | 马鞍山联洪合成材料有限公司 | A kind of composite magnetic attraction damping fin and its processing method |
| CN110422865A (en) * | 2019-08-13 | 2019-11-08 | 浙江钙科机械设备有限公司 | A kind of aerated bricks calcium oxide production technology |
| CN110467202A (en) * | 2019-07-12 | 2019-11-19 | 赵宁 | A kind of sodium hydroxide preparation process |
| CN111548651A (en) * | 2020-05-22 | 2020-08-18 | 李军祥 | Improved barite powder production method |
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| JP2007126333A (en) * | 2005-11-04 | 2007-05-24 | New Raimu Kenkyusha:Kk | Vaterite type disk-shaped calcium carbonate and its production method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163595A (en) * | 2017-05-31 | 2017-09-15 | 马鞍山联洪合成材料有限公司 | A kind of composite magnetic attraction damping fin and its processing method |
| CN110467202A (en) * | 2019-07-12 | 2019-11-19 | 赵宁 | A kind of sodium hydroxide preparation process |
| CN110422865A (en) * | 2019-08-13 | 2019-11-08 | 浙江钙科机械设备有限公司 | A kind of aerated bricks calcium oxide production technology |
| CN111548651A (en) * | 2020-05-22 | 2020-08-18 | 李军祥 | Improved barite powder production method |
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