CN109160877A - The production method of medical calcium lactate - Google Patents
The production method of medical calcium lactate Download PDFInfo
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- CN109160877A CN109160877A CN201811174128.4A CN201811174128A CN109160877A CN 109160877 A CN109160877 A CN 109160877A CN 201811174128 A CN201811174128 A CN 201811174128A CN 109160877 A CN109160877 A CN 109160877A
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- lactic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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Abstract
The invention discloses a kind of production methods of medical calcium lactate, comprising the following steps: 1) using food grade lactic acid as raw material, concentrated distillation obtains the lactic acid of resistance to thermal level；2) add water that calcium carbonate slurry is made with calcium carbonate, the lactic acid of resistance to thermal level is then added, heating stirring is reacted, until the pH of feed liquid is in 4.5-5.5；3) add water that calcium hydroxide slurry is made with calcium oxide, the feed liquid for then obtaining step 2 is mixed with, and is reacted, until the pH value of feed liquid is in 8.5-9.5；4) active carbon is added in the feed liquid that step 3) obtains and carries out adsorption bleaching, filtrate is once collected by filtration in rear stewing process, and the pH value for adjusting filtrate is 6.8-7.2, then through secondary filter, filtrate is through mist projection granulating；5) step 4) resulting material is sieved, then two dimension mixing, is most detected metal through metal detector afterwards and is rejected, obtains medical calcium lactate.The product color is pure white, and impurity content is low, and product purity is high, and yield can reach 99.5%, can be used as the medical material for drug of replenishing the calcium.
Description
Technical field
A kind of medical material technical field of the present invention, and in particular to production method of medical calcium lactate.
Background technique
Calcium lactate, chemical name ɑ-hydracrylic acid calcium, general pentahydrate, molecular formula are (CH3CHOHCOO)2Ca·5H2O,
Molecular weight is 308.3, is white particle or powder, and free from extraneous odour, micro- have efflorescence properties, is soluble in hot water, insoluble in ethyl alcohol, ether and
Chloroform.Calcium lactate has the characteristics that solubility is high, solution rate is fast, bioavailability is high, is a kind of excellent calcium supplement, as
In the production of medical material application calcium-supplementing preparation, it can be used for preventing and treating the generation of the diseases such as skeleton bulking disease, bone embrittlement,
And enhancing development.
CN200610124931.8 is related to the dry production partilce calcium lactate technique of spraying granulation.It uses spraying granulation dry
Machine is atomized calcium lactate solution, is dried, is pelletized, by calcium lactate solution in keeping warm mode using compressed air and hot-air
Under be pumped into spraying granulation drying machine, the downward ejection that nebulizes is mixed with compressed air, with hot air from bottom to top into
Particle is dried to after row heat exchange；And then at particle.The patent only discloses the method for liquid calcium lactate spray granulating and drying,
For a step of calcium lactate production, the formation of liquid calcium lactate is not described, technique is not comprehensive, can not judge to use this
The quality for the lactic acid calcium product that method obtains also is not illustrated in specification.
CN201410512647.2 is related to the production technology that a step chemical reaction prepares calcium lactate.This technique is with cheap and easily-available
Lactic acid and calcium carbonate be raw material, take water as a solvent, certain molar equivalent proportion, certain reaction temperature under the conditions of, double decomposition
Reaction obtains calcium lactate solution；A certain amount of ethyl alcohol, cooling and standings crystallization is added in calcium lactate solution, and ethanol washing crystallization is dried, done
It is dry, obtain refining calcium lactate finished product.The production technology of its calcium lactate announced crystallization, is added a certain amount of ethyl alcohol, although ethyl alcohol has
Certain volatility, but still it is not excluded for the residual in product there are alcohols material, it is also illustrated in specification.And in reality
Reaction process in lactic acid can not be reacted completely with calcium carbonate, there are defective workmanships.Method yield simultaneously using crystallization is not high,
Yield only reaches 87.2%.
CN201410061529.4 is related to a kind of production method of the L-calcium lactate of high features good taste of solubility, and innovative point exists
In: this method is in proportion to put into Pfansteihl and calcium gluconate in water, is heated to dissolved clarification；It is slowly added into a certain amount of
Calcium hydroxide adjusts pH to 5.4-6.7, Baume degrees 16-19；Active carbon decoloring is added into solution again, after filters pressing, spray drying
Screening, is packed and stored.Practical is the production of the mixture of calcium lactate and calcium gluconate.
CN201611125774.2 is related to technical field of medicine, discloses a kind of preparation method of calcium lactate tablet, former
Material is made of calcium lactate, dextrin, starch, magnesium stearate, medicinal 95% appropriate amount of ethanol.The patent is a kind of preparation of calcium lactate tablet
Method, raw material and production method, formula are different from present patent application.
CN201711455234.5 is related to a kind of method for preparing calcium lactate crystal, additionally provides a kind of by calcium lactate crystalline substance
The method that body produces the lactic acid of resistance to thermal level.Using calcium lactate fermentation solution as raw material, it is filtered and is concentrated, then cooling crystallization,
Wash calcium lactate crystal of the calcium lactate crystal twice to get purity for 99% or more mass percent.The patent uses calcium lactate
Fermentation liquid is raw material, and raw material impurity is more, it is necessary to is removed using the method for crystallization, but the method crystallized can not accomplish impurity
It completely removes, product still contains a small amount of carbohydrate, protein, volatile fat acid, and yield is not high, and this patent is equal
It does not hand over.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of production method of medical calcium lactate, what this method obtained
Calcium lactate color is pure white, and impurity content is low, and product purity is high, meets Chinese Pharmacopoeia 2015 editions requirements, can be used as drug of replenishing the calcium
Medical material.
The technical solution adopted by the present invention is that a kind of production method of medical calcium lactate, comprising the following steps:
1) using food grade lactic acid as raw material, concentrated distillation obtains the lactic acid of resistance to thermal level；
2) add water that calcium carbonate slurry is made with calcium carbonate, the lactic acid of resistance to thermal level is then added, heating stirring is reacted, until material
The pH of liquid is in 4.5-5.5；
3) add water that calcium hydroxide slurry is made with calcium oxide, the feed liquid for then obtaining step 2) is mixed with, and is carried out anti-
It answers, until the pH value of feed liquid is in 8.5-9.5；
4) active carbon is added in the feed liquid that step 3) obtains and carries out adsorption bleaching, filter is once collected by filtration in rear stewing process
Liquid, the pH value for adjusting filtrate is 6.8-7.2, then through secondary filter, filtrate is through mist projection granulating；
5) step 4) resulting material is sieved, then two dimension mixing, is most detected metal through metal detector afterwards and is rejected,
Obtain medical calcium lactate.
Further, the food grade lactic acid obtains resistance to thermal level cream by luwa evaporator concentration and short-range molecular distillation
Acid, wherein the mass concentration for the lactic acid of resistance to thermal level be 99% or more, lactic acid be heated to reflux at 180-200 DEG C 2 hours colorations≤
50APHA。
Further, the calcium carbonate and calcium oxide are food-grade.Meet national food safety standard food additives
Standard., calcium carbonate is preferable over molysite≤0.01%；Sulfate≤0.01%.
Further, the active carbon is injection-use activated carbon, and additional amount is the 0.2-0.5% of lactic acid quality；Absorption
The impurity such as pigment.Time of repose is 1.5-3 hours；First is that adsorbing activated carbon sufficiently；Second is that activated carbon is made to be sunken to tank bottom, concentrate
It is easy to form filtering layer on silk screen rapidly when activated carbon when releasing.At this point, the mass fraction of calcium lactate feed liquid is 33-38%.
Further, primary filtering uses filtering machine with horizontal blade；Calcium lactate feed liquid and active carbon are separated, and lactic acid is obtained
Calcium supernatant liquid；When adjusting pH, it is adjusted using the lactic acid of resistance to thermal level；Stud filter is used when secondary filter, is further gone
Except impurity.
Further, the filter medium of filtering machine with horizontal blade is wire mesh, and aperture is 280-320 mesh；Stud filtering
The aperture of the stud of device is 0.20-0.30 microns.
Further, it when mist projection granulating, is dried using hot-air, hot air temperature is 100-120 DEG C.By twice
It filters and adjusts the calcium lactate feed liquid of pH by pressure to mix in certain flow indentation spray drying device nozzle with compressed air
Synthesis is misty to be sprayed, and is dried to particle after carrying out heat exchange by the hot air of lower part from bottom to top.
Further, the material for being spray-dried completion is transported to high-order basin by air-flow, enters under the effect of gravity
It is sieved in screening machine, the aperture of sieve used is 40-60 mesh；The material that screening is completed is transported to mixing apparatus by air-flow
Interior, the time of two dimension mixing is 10-15min.Two dimension is mixed into the mixing of product single batch, with a batch uniform in quality.
Further, the mixed calcium lactate solid material of two dimension is transported to high-order basin by air-flow, in gravity
It is lower to enter duct type metal detector and flush trimmer, it detects metal and rejects；Eliminate the metallic foreign body in product.The metal
Survey meter is duct type metal detector.Obtained lactic acid calcium product can be packed as needed.
Chemical equation of the present invention are as follows:
2CH3CHOHCOOH+CaCO3=(CH3CHOHCOO)2Ca+CO2+H2O
2CH3CHOHCOOH+Ca(OH)2=(CH3CHOHCOO)2Ca+2H2O
(CH3CHOHCOO)2Ca+2H2O——(CH3CHOHCOO)2Ca·5H2O
The present invention activated carbon adsorption, standing, filtering, spray drying, screening, mixes feed purification, raw material selection and reaction
Close, metallic foreign body detection and reject, the entire production process such as packaging has carried out the complete explanation of system.It is comprehensively careful
Elaborate a kind of production method of pharmaceutical grade calcium lactate, purity higher carbonic acid low using high-purity lactic acid and impurity content
Calcium is reacted, from the introducing of the impurity contents such as source control carbohydrate, protein, fatty acid.Using horizontal blade wire mesh
Filtering with stud can remove 0.3 micron of visible foreign below, guarantee the clear of calcium lactate final mean annual increment solution.Using metal tube
Road detection and rejecting step, can remove metallic foreign body in finished product calcium lactate, meet the external requirement to product.
The present invention has the following advantages that and effect:
1, calcium lactate products material lactic acid first carries out purifying and prepares the lactic acid of resistance to thermal level, then carries out instead with high quality calcium carbonate
It answers, raw material is avoided to introduce more impurity and cause product physical and chemical index unqualified；Material purity is high, and impurity content is low, is allowed to
Product impurity content is low.
2, it is once filtered using horizontal blade wire mesh and stud filter carries out secondary filter, can remove all
Active carbon and visible foreign.
3, it increases metallic conduit detection and rejects step, can remove the metallic foreign body in product.Product purity is high, impurity
Content is low, meets Chinese Pharmacopoeia 2015 editions requirements, can be used as the medical material for drug of replenishing the calcium.
Specific embodiment
Below with reference to embodiment, the present invention is furture elucidated.
Embodiment 1:
1, lactic acid purifies: food grade lactic acid is concentrated by knifing and short-range molecular distillation, obtains the resistance to thermal level cream of sufficient amount
Acid, concentration are 99.9% mass ratio；
2, calcium carbonate is sized mixing: in 2m3Blend tank in be added 900KG purified water, under stirring be added meet food
The calcium carbonate raw material 250KG of product additive calcium carbonate national standard is mixed；
3, it is reacted with lactic acid: in 5m3In reactor tank, the purified lactic acid of 500KG (99.9%), collet is added
The heating of 0.15MPa steam, is all slowly added to calcium carbonate serosity in 85-95 DEG C of temperature range, under stirring and is reacted,
Reaction time 220 minutes, after the completion material liquid pH value be 4.9,92 DEG C of solution temperature；
4, calcium oxide is sized mixing: the purified water of 100KG being added in blend tank, is added under stirring and meets food addition
The calcium oxide raw material 25KG of agent calcium oxide national standard mixes, obtains calcium hydroxide slurry；
5 and calcium hydroxide reaction: by the calcium hydroxide slurry in blend tank, being slowly added to the reaction of above-mentioned reactor tank
In liquid, and keep temperature of charge in 85-95 DEG C of temperature range, when the pH value of reaction solution is 8.6, visual response is complete, obtains
1722KG calcium lactate solution；
6, activated carbon adsorption: 767 needle-use activated carbon 7KG are added after the reaction was completed, in feed liquid, stir evenly, adsorpting pigment
Equal impurity；
7, stand: the feed liquid that stirs evenly that active carbon is added stops stirring, stands 2 hours, at this time calcium lactate feed liquid
Mass fraction is 35.0%；
8, horizontal blade filters: feed liquid is pumped into horizontal blade filter, and calcium lactate feed liquid and active carbon are separated, and is obtained
Calcium lactate supernatant liquid；
9, adjust pH value: it is 7.1 that the lactic acid of 4KG after purification is added in feed liquid and adjusts solution ph；
10, stud filters: in the calcium lactate feed liquid indentation stud filter regulated, further removing impurity；
11, spraying granulation is dry: the calcium lactate feed liquid by filtering and adjusting pH twice is sent into the flow of 100L/H
The ejection that nebulizes is mixed with 0.3MPa clean compressed air in spray drying device nozzle, with the hot-air by lower part from bottom to top
(100-120 DEG C) contact dehydrates after carrying out heat exchange, obtains five water lactic acid calcium particle of 850KG；
12, sieve: the material for being spray-dried completion is transported to high-order basin by air-flow, enters sieve under the effect of gravity
It is sieved in extension set, the aperture of sieve is 60 mesh；
13, mix: the material for sieving completion is transported in mixing apparatus by air-flow, two dimension mixing 15 minutes；
14, metal detection and rejecting: calcium lactate solid material is transported to high-order basin by air-flow, under the effect of gravity into
Enter duct type metal detection and flush trimmer, detect metal and rejects；
15, pack: the material for mixing completion enters packaging facilities and is packed automatically.
Embodiment 2:
1, lactic acid purifies: food grade lactic acid is concentrated by knifing and short-range molecular distillation, obtains the resistance to thermal level cream of sufficient amount
Acid, concentration are 99.9% mass ratio；
2, calcium carbonate is sized mixing: in 2m3Blend tank in be added 1350KG purified water, under stirring be added meet food
The calcium carbonate raw material 375KG of product additive calcium carbonate national standard is mixed；
3, it is reacted with lactic acid: in 5m3In reactor tank, the purified lactic acid of 750KG (99.9%), collet is added
The heating of 0.15MPa steam, is all slowly added to calcium carbonate serosity in 85-95 DEG C of temperature range, under stirring and is reacted,
Reaction time 240 minutes, after the completion material liquid pH value be 4.7,93 DEG C of solution temperature；
4, calcium oxide is sized mixing: the purified water of 150KG being added in blend tank, is added under stirring and meets food addition
The calcium oxide raw material 40KG of agent calcium oxide national standard mixes, obtains calcium hydroxide slurry；
5 and calcium hydroxide reaction: by the calcium hydroxide slurry in blend tank, being slowly added to the reaction of above-mentioned reactor tank
In liquid, and keep temperature of charge in 85-95 DEG C of temperature range, when the pH value of reaction solution is 8.8, visual response is complete, obtains
2622KG calcium lactate solution；
6, activated carbon adsorption: 767 needle-use activated carbon 10KG are added after the reaction was completed, in feed liquid, stir evenly, adsorpting pigment
Equal impurity；
7, stand: the feed liquid that stirs evenly that active carbon is added stops stirring, stands 2 hours, at this time calcium lactate feed liquid
Mass fraction is 35.6%；
8, horizontal blade filters: feed liquid is pumped into horizontal blade filter, and calcium lactate feed liquid and active carbon are separated, and is obtained
Calcium lactate supernatant liquid；
9, adjust pH value: it is 7.2 that the lactic acid of 8KG after purification is added in feed liquid and adjusts solution ph；
10, stud filters: in the calcium lactate feed liquid indentation stud filter regulated, further removing impurity；
11, spraying granulation is dry: the calcium lactate feed liquid by filtering and adjusting pH twice is sent into the flow of 100L/H
The ejection that nebulizes is mixed with 0.3MPa clean compressed air in spray drying device nozzle, with the hot-air by lower part from bottom to top
(100-120 DEG C) contact dehydrates after carrying out heat exchange, obtains five water lactic acid calcium particle of 1305KG；
12, sieve: the material for being spray-dried completion is transported to high-order basin by air-flow, enters sieve under the effect of gravity
It is sieved in extension set, the aperture of sieve is 60 mesh；
13, mix: the material for sieving completion is transported in mixing apparatus by air-flow, two dimension mixing 15 minutes；
14, metal detection and rejecting: calcium lactate solid material is transported to high-order basin by air-flow, under the effect of gravity into
Enter duct type metal detection and flush trimmer, detect metal and rejects；
15, pack: the material for mixing completion enters packaging facilities and is packed automatically.
Embodiment 3:
1, lactic acid purifies: food grade lactic acid is concentrated by knifing and short-range molecular distillation, obtains the resistance to thermal level cream of sufficient amount
Acid, concentration are 99.9% mass ratio；
2, calcium carbonate is sized mixing: in 2m3Blend tank in be added 1350KG purified water, under stirring be added meet food
The calcium carbonate raw material 375KG of product additive calcium carbonate national standard is mixed；
3, it is reacted with lactic acid: in 5m3In reactor tank, the purified lactic acid of 750KG (99.9%), collet is added
The heating of 0.15MPa steam, is all slowly added to calcium carbonate serosity in 85-95 DEG C of temperature range, under stirring and is reacted,
Reaction time 240 minutes, after the completion material liquid pH value be 4.6,94 DEG C of solution temperature；
4, calcium oxide is sized mixing: the purified water of 150KG being added in blend tank, is added under stirring and meets food addition
The calcium oxide raw material 40KG of agent calcium oxide national standard mixes, obtains calcium hydroxide slurry；
5 and calcium hydroxide reaction: by the calcium hydroxide slurry in blend tank, being slowly added to the reaction of above-mentioned reactor tank
In liquid, and keep temperature of charge in 85-95 DEG C of temperature range, when the pH value of reaction solution is 9.0, visual response is complete, obtains
2615KG calcium lactate solution；
6, activated carbon adsorption: 767 needle-use activated carbon 10KG are added after the reaction was completed, in feed liquid, stir evenly, adsorpting pigment
Equal impurity；
7, stand: the feed liquid that stirs evenly that active carbon is added stops stirring, stands 3 hours, at this time calcium lactate feed liquid
Mass fraction is 35.8%；
8, horizontal blade filters: feed liquid is pumped into horizontal blade filter, and calcium lactate feed liquid and active carbon are separated, and is obtained
Calcium lactate supernatant liquid；
9, adjust pH value: it is 7.2 that the lactic acid of 5.4KG after purification is added in feed liquid and adjusts solution ph；
10, stud filters: in the calcium lactate feed liquid indentation stud filter regulated, further removing impurity；
11, spraying granulation is dry: the calcium lactate feed liquid by filtering and adjusting pH twice is sent into the flow of 100L/H
The ejection that nebulizes is mixed with 0.3MPa clean compressed air in spray drying device nozzle, with the hot-air by lower part from bottom to top
(100-120 DEG C) contact dehydrates after carrying out heat exchange, obtains five water lactic acid calcium particle of 1300KG；
12, sieve: the material for being spray-dried completion is transported to high-order basin by air-flow, enters sieve under the effect of gravity
It is sieved in extension set, the aperture of sieve is 60 mesh；
13, mix: the material for sieving completion is transported in mixing apparatus by air-flow, two dimension mixing 15 minutes；
14, metal detection and rejecting: calcium lactate solid material is transported to high-order basin by air-flow, under the effect of gravity into
Enter duct type metal detection and flush trimmer, detect metal and rejects；
15, pack: the material for mixing completion enters packaging facilities and is packed automatically.
Product quality, purity and impurity content detection data in above-described embodiment is as shown in table 1 below.
Table 1
Illustrate: band " * " detection is limited to 0.0001%.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this hair
Bright protection scope should be with the technical solution of claim record, technical characteristic in the technical solution recorded including claim
Equivalents are protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.
Claims (9)
1. a kind of production method of medical calcium lactate, which comprises the following steps:
1) using food grade lactic acid as raw material, concentrated distillation obtains the lactic acid of resistance to thermal level；
2) adding water that calcium carbonate slurry is made with calcium carbonate, the lactic acid of resistance to thermal level is then added, heating stirring is reacted, until feed liquid
PH is in 4.5-5.5；
3) add water that calcium hydroxide slurry is made with calcium oxide, the feed liquid for then obtaining step 2 is mixed with, it is reacted, until
The pH value of feed liquid is in 8.5-9.5；
4) active carbon is added in the feed liquid that step 3) obtains and carries out adsorption bleaching, filtrate is once collected by filtration in rear stewing process, adjusts
The pH value of entire filter liquid is 6.8-7.2, then through secondary filter, filtrate is through mist projection granulating；
5) step 4) resulting material is sieved, then two dimension mixing, is most detected metal through metal detector afterwards and is rejected, obtains
Medical calcium lactate.
2. according to the method described in claim 1, it is characterized by: the food grade lactic acid by luwa evaporator concentration and it is short
Journey molecular distillation obtains the lactic acid of resistance to thermal level, wherein the mass concentration for the lactic acid of resistance to thermal level is 99% or more, lactic acid adds at 180-200 DEG C
2 hours coloration≤50APHA of heat reflux.
3. according to the method described in claim 1, it is characterized by: the calcium carbonate and calcium oxide are food-grade.
4. according to the method described in claim 1, additional amount is it is characterized by: the active carbon is injection-use activated carbon
The 0.2-0.5% of lactic acid quality；Time of repose is 1.5-3 hours.
5. according to the method described in claim 1, it is characterized by: primary filtering uses filtering machine with horizontal blade；When adjusting pH,
It is adjusted using the lactic acid of resistance to thermal level；Stud filter is used when secondary filter.
6. according to the method described in claim 5, it is characterized by: the filter medium of filtering machine with horizontal blade be wire mesh,
Aperture is 280-320 mesh；The aperture of the stud of stud filter is 0.20-0.30 microns.
7. according to the method described in claim 1, it is characterized by: being dried using hot-air, hot-air when mist projection granulating
Temperature is 100-120 DEG C.
8. according to the method described in claim 1, it is characterized by: the aperture of sieve used is 40-60 mesh when screening；Two dimension is mixed
The time of conjunction is 10-15min.
9. according to the method described in claim 1, it is characterized by: the metal detector is duct type metal detector.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262266A (en) * | 2022-01-12 | 2022-04-01 | 中农科学研究院(广州)有限公司 | Preparation method of anhydrous calcium lactate particles |
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Application publication date: 20190108 |
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