CN106395877A - Preparation process of pure natural nano-ultrafine calcium powders - Google Patents
Preparation process of pure natural nano-ultrafine calcium powders Download PDFInfo
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- CN106395877A CN106395877A CN201610784457.5A CN201610784457A CN106395877A CN 106395877 A CN106395877 A CN 106395877A CN 201610784457 A CN201610784457 A CN 201610784457A CN 106395877 A CN106395877 A CN 106395877A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
- C01F11/12—Oxides or hydroxides from silicates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
- A61K33/08—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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Abstract
The invention provides a preparation process of pure natural nano-ultrafine calcium powders. The preparation process comprises the steps of primary stirring, secondary stirring and third stirring. Based on the preparation process, the production efficiency of calcium powders is improved and the labor time is reduced. Meanwhile, the cost of calcium powders is reduced. When prepared pure natural nano-ultrafine calcium powders are applied to a rubber product, the tensile strength of the rubber product can be up to 14. 8 MPa, and the breaking elongation rate thereof is up to 620%. Meanwhile, the tearing strength of the rubber product reaches 35-38 KN/m. When prepared pure natural nano-ultrafine calcium powders are applied to a pharmaceutical product, the bone mass can be effectively reduced and the recovery rate of osteoporosis patients is up to 84-96%. The symptoms of osteoporosis are greatly alleviated.
Description
Technical field
The present invention relates to a kind of preparation technology of calcium powder, specifically, it is related to a kind of system of pure natural nanometer ultra micro calcium powder
Standby technique, belongs to calcium powder preparing technical field.
Background technology
Calcium is the crystal that is silvery white in color under a kind of metallic element, room temperature.The skeleton of animal, Concha Meretricis Seu Cyclinae, eggshell all contain Calcium Carbonate.
Calcium is the most mineral of body burden, has 99% calcium to be present in skeleton and tooth, and 1% is present in our blood,
It is referred to as blood calcium, human body calcium deficiency can cause osteoporosis.Display is investigated according to Chinese Medical Association：Chinese calcium is average daily at present
Intake is only 400 milligrams about, and the daily calcium magnitude of recruitment of Chinese Medical Association's suggestion is 800-1000 milligram.In order to keep blood
The concentration of calcium in liquid, body will be released the calcium in bone and be added in blood, cause the loss of calcium in skeleton, this feelings
Condition we be called body calcium deficiency.The supplement of calcium can be realized by edible calcium containing food, calcic health product and calcic medicine,
But often assimilation effect is very poor for the mode of this supplementary calcium, do not reach the effect for the treatment of body calcium deficiency.And in prior art, calcium
It is not very universal for being applied to rubber materials, adds calcium in rubber product, and the performance of rubber product does not change；
Meanwhile, in prior art, it is low to prepare calcium powder efficiency, and high cost is lost time more.
In summary, prior art there will naturally be inconvenience and defect in actual use, it is therefore necessary to being improved.
Content of the invention
The technical problem to be solved in the present invention is for not enough above, provides a kind of preparation of pure natural nanometer ultra micro calcium powder
Technique, can improve the production efficiency of calcium powder, decrease labor time, reduce calcium powder cost simultaneously；The present invention is used for rubber
After product, up to 14.8MPa, up to 620%, tearing strength reaches 35-38KN/m to elongation at break to the tensile strength of rubber product；
The present invention is used in medical product, can effectively reduce bone-loss, and sufferers of osteoporosis face cure rate is 84-96%, greatly
Alleviate osteoporotic symptom.
For solving above technical problem, the present invention employs the following technical solutions：A kind of system of pure natural nanometer ultra micro calcium powder
Standby technique, including once stirring, secondary stirring and triple mixing.
It is below the preferred version of the present invention：
A described whipping step is：
Will pulverize after calcite add the anaerobic pond containing activated sludge in, additions parts by weight be 25-35 part water,
15-25 part Herba bromi japonici bar extract extract, 1-3 part glucose and 7-9 part ethanol are stirred, and control temperature to be 60 DEG C, rotating speed
For 200-250 rev/min, mixing time is 36-48 hour.
Described secondary stirring step is：
After once stirring terminates, adjustment rotating speed is 700-780 rev/min, is again stirring for, and mixing time is 1-2 hour.
In described triple mixing step：
Add the dilute sulfuric acid that 500 milliliters of concentration are 0.7mol/L, improve temperature to 100 DEG C, after stirring 20-30 minute, quiet
Put 10-20 minute, wash 1-3 time in latex deionized water again, obtain the Crystallization of Gypsum compound of purification.
After Crystallization of Gypsum compound heating and melting, melt thing in add weight portion be 20-30 part water and
Weight portion is the barium hydroxide of 10-20 part, controls rotating speed to be 800 revs/min, stirs 20 minutes, filters, solution after filtration
Middle addition parts by weight are 20 parts of sodium hydroxide, and stirring obtains the precipitate based on Ca (OH) 2.
Also include pulverising step, in described pulverising step：
Pulverizing 40-60 minute in pulverizer will be placed in, to particle diameter after the Calcite Surface natural air drying of removal surface sludge
For 0.5-1cm.
Also include selection step, in described selection step：
Choose the calcite that weight portion is 5-7 part, carry out soaking after 10 minutes using the clear water for 6.8-7.0 for the pH, use
PH rinses for the clear water that 6.8-7.0 flows.
Also include grinding steps and baking step,
In described grinding steps：
Add 1-2 part water to be ground, obtain the water mill oleo stock based on Ca (OH) 2；
In described baking step：
Water mill oleo stock is ground to particle diameter as being placed in after 0.1-0.5um in the dehydrator that temperature is 200-220 DEG C
Row is dried, and obtains product.
The effective ingredient of described Herba bromi japonici bar extract is xylose, and the content of described xylose is 58.8-63.4%.
The extraction step of described Herba bromi japonici bar extract is：
(1) from water content, the Herba bromi japonici bar raw material for 65%-70% is cut, and being cut to length is 2-3cm, takes 50 parts
Standby；
(2) 250 parts of water, steaming and decocting 2 hours under the conditions of temperature is for 100-105 DEG C are added；
(3) water washing being 40 DEG C with temperature 6 times；
(4) 150 parts of concentration of addition are 0.70% sulfuric acid solution, and be hydrolyzed under the conditions of temperature is for 110-112 DEG C place
Reason, reaches 13-15% to xylose concentration, obtains xylose.
After the present invention adopts above technical scheme, compared with prior art, there is advantages below：
(1) present invention substantially increases the production efficiency of calcium powder, decreases labor time, reduces calcium powder cost simultaneously；
(2) after the present invention is used for rubber product, the tensile strength of rubber product up to 14.8MPa, elongation at break up to
620%, tearing strength reaches 35-38KN/m；
(3) present invention is used in medical product, can effectively reduce bone-loss, sufferers of osteoporosis face cure rate is
84-96%, greatly alleviates osteoporotic symptom.
Specific embodiment
In order to be more clearly understood to the technical characteristic of the present invention, purpose and effect, now to the present invention's as directed
Specific embodiment.
Embodiment 1, a kind of preparation technology of pure natural nanometer ultra micro calcium powder, comprise the following steps：
A selection
Choose the calcite that weight portion is 5 parts, carry out soaking after 10 minutes using the clear water that pH is 6.8, the use of pH is 6.8
The clear water of flowing rinses one time, removes surface sludge；
B pulverizes
It is placed in pulverizing 40 minutes in pulverizer after removing the Calcite Surface natural air drying of surface sludge in step A, extremely
Particle diameter is 0.5-1cm；
C once stirs
Calcite after pulverizing adds in the anaerobic pond containing activated sludge, adds parts by weight to be 25 parts of water, 15 parts
Herba bromi japonici bar extract extract, 1 part of glucose and 7 parts of ethanol are stirred, and control temperature to be 60 DEG C, rotating speed is 200 revs/min
Clock, mixing time is 36 hours；
The effective ingredient of described Herba bromi japonici bar extract is xylose, and the content of described xylose is 58.8-63.4%；
The extraction step of described Herba bromi japonici bar extract is：
(1) from water content, the Herba bromi japonici bar raw material for 65%-70% is cut, and being cut to length is 2-3cm, takes 50 parts
Standby；
(2) 250 parts of water, steaming and decocting 2 hours under the conditions of temperature is for 100-105 DEG C are added；
(3) water washing being 40 DEG C with temperature 6 times；
(4) 150 parts of concentration of addition are 0.70% sulfuric acid solution, and be hydrolyzed under the conditions of temperature is for 110-112 DEG C place
Reason, reaches 13-15% to xylose concentration, obtains xylose；
D secondary stirring
After above-mentioned step C terminates, adjustment rotating speed is 700 revs/min, is again stirring for, and mixing time is 1 hour；
F stands
After above-mentioned D step terminates, water outlet is stood 6 hours, the clear liquor of filtration separation；
G triple mixing
The dilute sulfuric acid that 500 milliliters of concentration are 0.7mol/L will be added in the clear liquor of gained in step F, improve temperature extremely
100 DEG C, after stirring 20 minutes, stand 10 minutes, wash 1 time in latex deionized water again, obtain the calcium sulphate dihydrate of purification
Crystalline compounds；After Crystallization of Gypsum compound heating and melting, melt thing in add weight portion be 20 parts water and
Weight portion is 10 parts of barium hydroxide, controls rotating speed to be 800 revs/min, stirs 20 minutes, filters, in solution after filtration
Add the sodium hydroxide that parts by weight are 20 parts, stirring, obtain the precipitate based on Ca (OH) 2；
H grinds
The precipitate of gained in step G is added 1 water to be ground, obtains the water mill oleo stock based on Ca (OH) 2；
I is dried
The water mill oleo stock of gained in step H is ground to particle diameter as being placed in the baking that temperature is 200 DEG C after 0.1-0.5um
Dried in dry machine, obtained product.
Embodiment 2, a kind of preparation technology of pure natural nanometer ultra micro calcium powder, comprise the following steps：
A selection
Choose the calcite that weight portion is 6 parts, carry out soaking after 10 minutes using the clear water that pH is 6.9, the use of pH is 6.9
The clear water of flowing rinses one time, removes surface sludge；
B pulverizes
It is placed in pulverizing 50 minutes in pulverizer after removing the Calcite Surface natural air drying of surface sludge in step A, extremely
Particle diameter is 0.5-1Gm；
C once stirs
Calcite after pulverizing adds in the anaerobic pond containing activated sludge, adds parts by weight to be 30 parts of water, 20 parts
Herba bromi japonici bar extract extract, 2 parts of glucoses and 8 parts of ethanol are stirred, and control temperature to be 60 DEG C, rotating speed is 225 revs/min
Clock, mixing time is 42 hours；
The effective ingredient of described Herba bromi japonici bar extract is xylose, and the content of described xylose is 58.8-63.4%；
The extraction step of described Herba bromi japonici bar extract is：
(1) from water content, the Herba bromi japonici bar raw material for 65%-70% is cut, and being cut to length is 2-3cm, takes 50 parts
Standby；
(2) 250 parts of water, steaming and decocting 2 hours under the conditions of temperature is for 100-105 DEG C are added；
(3) water washing being 40 DEG C with temperature 6 times；
(4) 150 parts of concentration of addition are 0.70% sulfuric acid solution, and be hydrolyzed under the conditions of temperature is for 110-112 DEG C place
Reason, reaches 13-15% to xylose concentration, obtains xylose；
D secondary stirring
After above-mentioned step C terminates, adjustment rotating speed is 740 revs/min, is again stirring for, and mixing time is 1.5 hours；
F stands
After above-mentioned D step terminates, water outlet is stood 7 hours, the clear liquor of filtration separation；
G triple mixing
The dilute sulfuric acid that 500 milliliters of concentration are 0.7mol/L will be added in the clear liquor of gained in step F, improve temperature extremely
100 DEG C, after stirring 25 minutes, stand 15 minutes, wash 2 times in latex deionized water again, obtain the calcium sulphate dihydrate of purification
Crystalline compounds；After Crystallization of Gypsum compound heating and melting, melt thing in add weight portion be 25 parts water and
Weight portion is 15 parts of barium hydroxide, controls rotating speed to be 800 revs/min, stirs 20 minutes, filters, in solution after filtration
Add the sodium hydroxide that parts by weight are 20 parts, stirring, obtain the precipitate based on Ca (OH) 2；
H grinds
The precipitate of gained in step G is added 1.5 parts of water to be ground, obtains the water mill oleo stock based on Ca (OH) 2；
I is dried
The water mill oleo stock of gained in step H is ground to particle diameter as being placed in the baking that temperature is 210 DEG C after 0.1-0.5um
Dried in dry machine, obtained product.
Embodiment 3, a kind of preparation technology of pure natural nanometer ultra micro calcium powder, comprise the following steps：
A selection
Choose the calcite that weight portion is 7 parts, carry out soaking after 10 minutes using the clear water that pH is 7.0, the use of pH is 7.0
The clear water of flowing rinses one time, removes surface sludge；
B pulverizes
It is placed in pulverizing 60 minutes in pulverizer after removing the Calcite Surface natural air drying of surface sludge in step A, extremely
Particle diameter is 0.5-1cm；
C once stirs
Calcite after pulverizing adds in the anaerobic pond containing activated sludge, adds parts by weight to be 35 parts of water, 25 parts
Herba bromi japonici bar extract extract, 3 parts of glucoses and 9 parts of ethanol are stirred, and control temperature to be 60 DEG C, rotating speed is 250 revs/min
Clock, mixing time is 48 hours；
The effective ingredient of described Herba bromi japonici bar extract is xylose, and the content of described xylose is 58.8-63.4%；
The extraction step of described Herba bromi japonici bar extract is：
(1) from water content, the Herba bromi japonici bar raw material for 65%-70% is cut, and being cut to length is 2-3cm, takes 50 parts
Standby；
(2) 250 parts of water, steaming and decocting 2 hours under the conditions of temperature is for 100-105 DEG C are added；
(3) water washing being 40 DEG C with temperature 6 times；
(4) 150 parts of concentration of addition are 0.70% sulfuric acid solution, and be hydrolyzed under the conditions of temperature is for 110-112 DEG C place
Reason, reaches 13-15% to xylose concentration, obtains xylose；
D secondary stirring
After above-mentioned step C terminates, adjustment rotating speed is 780 revs/min, is again stirring for, and mixing time is 2 hours；
F stands
After above-mentioned D step terminates, water outlet is stood 8 hours, the clear liquor of filtration separation；
G triple mixing
The dilute sulfuric acid that 500 milliliters of concentration are 0.7mol/L will be added in the clear liquor of gained in step F, improve temperature extremely
100 DEG C, after stirring 30 minutes, stand 20 minutes, wash 3 times in latex deionized water again, obtain the calcium sulphate dihydrate of purification
Crystalline compounds；After Crystallization of Gypsum compound heating and melting, melt thing in add weight portion be 30 parts water and
Weight portion is 20 parts of barium hydroxide, controls rotating speed to be 800 revs/min, stirs 20 minutes, filters, in solution after filtration
Add the sodium hydroxide that parts by weight are 20 parts, stirring, obtain the precipitate based on Ca (OH) 2；
H grinds
The precipitate of gained in step G is added 2 parts of water to be ground, obtains the water mill oleo stock based on Ca (OH) 2；
I is dried
The water mill oleo stock of gained in step H is ground to particle diameter as being placed in the baking that temperature is 220 DEG C after 0.1-0.5um
Dried in dry machine, obtained product.
Testing result：
(1) present invention substantially increases the production efficiency of calcium powder, decreases labor time, reduces calcium powder cost simultaneously；
(2) after the present invention is used for rubber product, the tensile strength of rubber product up to 14.8MPa, elongation at break up to
620%, tearing strength reaches 35-38KN/m, and specific targets are shown in Table 1；
Table 1
Comparison：Not using the rubber product of ultra micro calcium powder
(3) present invention is used in medical product, can effectively reduce bone-loss, greatly alleviate osteoporotic
Symptom.From 100 sufferers of osteoporosis face, T value ＜ -2.5, it is divided into four groups, every group of 25 people, go back for first group in addition to normal diet
The edible medicinal product adding embodiment 1 ultra micro calcium powder；Second group of also edible interpolation embodiment 2 micro-calcium in addition to normal diet
The medicinal product of powder；The 3rd group of also edible medicinal product adding embodiment 3 ultra micro calcium powder in addition to normal diet；4th group is
Matched group, except normal diet does not eat any medicinal product containing ultra micro calcium powder；Test 7 days, 14 days, 21 days, 28 days when respectively
Carry out detecting osteoporosises T value in four group memberships, sufferers of osteoporosis face cure rate is 84-96%, specific targets are shown in Table 2；
Table 2 osteoporosises T value ＜ 2.5 demographic
Comparison：Normal diet does not eat any medicinal product containing ultra micro calcium powder
The above is the citing of best mode for carrying out the invention, and it is common that the part wherein do not addressed in detail is this area
The common knowledge of technical staff.Protection scope of the present invention is defined by the content of claim, any technology based on the present invention
The equivalent transformation enlightening and carrying out, also within protection scope of the present invention.
Claims (10)
1. a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Including once stirring, secondary stirring and three times
Stirring.
2. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Described once stir
Mixing step is：
Calcite after pulverizing is added in the anaerobic pond containing activated sludge, adds parts by weight to be 25-35 part water, 15-25
Part Herba bromi japonici bar extract extract, 1-3 part glucose and 7-9 part ethanol are stirred, and control temperature to be 60 DEG C, and rotating speed is 200-
250 revs/min, mixing time is 36-48 hour.
3. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Described secondary stir
Mixing step is：
After once stirring terminates, adjustment rotating speed is 700-780 rev/min, is again stirring for, and mixing time is 1-2 hour.
4. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Stir for described three times
Mix in step：
Add the dilute sulfuric acid that 500 milliliters of concentration are 0.7mol/L, improve temperature to 100 DEG C, after stirring 20-30 minute, stand 10-
20 minutes, wash 1-3 time in latex deionized water again, obtain the Crystallization of Gypsum compound of purification.
5. as claimed in claim 4 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：
After Crystallization of Gypsum compound heating and melting, add the water that weight portion is 20-30 part and weight in melting thing
Part is the barium hydroxide of 10-20 part, controls rotating speed to be 800 revs/min, stirs 20 minutes, and filtration adds in solution after filtration
Enter the sodium hydroxide that parts by weight are 20 parts, stirring, obtain the precipitate based on Ca (OH) 2.
6. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Also include pulverizing
Step, in described pulverising step：
Pulverizing 40-60 minute in pulverizer will be placed in after the Calcite Surface natural air drying of removal surface sludge, to particle diameter be
0.5-1cm.
7. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Also include selection
Step, in described selection step：
Choose the calcite that weight portion is 5-7 part, carry out soaking after 10 minutes using the clear water for 6.8-7.0 for the pH, using pH be
The clear water of 6.8-7.0 flowing rinses.
8. as claimed in claim 1 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Also include grinding
Step and baking step,
In described grinding steps：
Add 1-2 part water to be ground, obtain the water mill oleo stock based on Ca (OH) 2；
In described baking step：
Water mill oleo stock is ground to particle diameter being dried for being placed in after 0.1-0.5um in the dehydrator that temperature is 200-220 DEG C
Dry, obtain product.
9. as claimed in claim 2 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：Described Herba bromi japonici bar
The effective ingredient of extract is xylose, and the content of described xylose is 58.8-63.4%.
10. as claimed in claim 2 a kind of preparation technology of pure natural nanometer ultra micro calcium powder it is characterised in that：
The extraction step of described Herba bromi japonici bar extract is：
(1) from water content, the Herba bromi japonici bar raw material for 65%-70% is cut, be cut to length be 2-3cm, take 50 parts standby
With；
(2) 250 parts of water, steaming and decocting 2 hours under the conditions of temperature is for 100-105 DEG C are added；
(3) water washing being 40 DEG C with temperature 6 times；
(4) 150 parts of concentration of addition are 0.70% sulfuric acid solution, and be hydrolyzed under the conditions of temperature is for 110-112 DEG C process, extremely
Xylose concentration reaches 13-15%, obtains xylose.
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| CN104176757A (en) * | 2014-08-08 | 2014-12-03 | 石棉县亿欣钙业有限责任公司 | Light calcium carbonate suspension calcining process |
| CN104495900A (en) * | 2014-12-01 | 2015-04-08 | 南昌航空大学 | Method for preparing nanometer calcium carbonate powder by mechanochemical method of shells |
| CN104828851A (en) * | 2015-04-21 | 2015-08-12 | 南通南辉电子材料股份有限公司 | Production method and production device of calcium sulphate dihydrate |
| CN105197976A (en) * | 2015-10-19 | 2015-12-30 | 高大元 | Preparation method of nano calcium carbonate powder |
| CN105417569A (en) * | 2015-12-28 | 2016-03-23 | 常熟市宏宇钙化物有限公司 | Preparation method of rodlike nano-calcium carbonate |
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