CN112320779A - Hydroxyapatite forming method and hydroxyapatite application - Google Patents
Hydroxyapatite forming method and hydroxyapatite application Download PDFInfo
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- CN112320779A CN112320779A CN202011321184.3A CN202011321184A CN112320779A CN 112320779 A CN112320779 A CN 112320779A CN 202011321184 A CN202011321184 A CN 202011321184A CN 112320779 A CN112320779 A CN 112320779A
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- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims abstract description 33
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 248
- 238000006243 chemical reaction Methods 0.000 claims abstract description 229
- 239000000203 mixture Substances 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 238000004140 cleaning Methods 0.000 claims abstract description 35
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims abstract description 17
- 235000019838 diammonium phosphate Nutrition 0.000 claims abstract description 17
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 16
- 239000010440 gypsum Substances 0.000 claims abstract description 16
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 16
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000001110 calcium chloride Substances 0.000 claims abstract description 15
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 15
- 239000008267 milk Substances 0.000 claims abstract description 15
- 210000004080 milk Anatomy 0.000 claims abstract description 15
- 235000013336 milk Nutrition 0.000 claims abstract description 15
- 239000008213 purified water Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000005696 Diammonium phosphate Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000376 reactant Substances 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 210000000988 bone and bone Anatomy 0.000 claims description 4
- 230000017423 tissue regeneration Effects 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002316 cosmetic surgery Methods 0.000 description 2
- 238000001727 in vivo Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- 206010005963 Bone formation increased Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000000316 bone substitute Substances 0.000 description 1
- 229940069978 calcium supplement Drugs 0.000 description 1
- 238000011097 chromatography purification Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/112—Phosphorus-containing compounds, e.g. phosphates, phosphonates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Inorganic Chemistry (AREA)
- Dermatology (AREA)
- General Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
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Abstract
The invention discloses a forming method of hydroxyapatite, which comprises the following steps: s1: preparing the following raw materials in parts by weight: 15-20 parts of calcium carbonate, 10-15 parts of gypsum, 150-250 parts of purified water, 20-25 parts of calcium chloride, 15-20 parts of milk, 10-15 parts of diammonium phosphate solution and 40-60 parts of strong ammonia water; s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, and respectively marking the interiors of the two reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 10-15min, so as to obtain a first mixture; preparing two stirring reaction kettles, and respectively cleaning the insides of the two stirring reaction kettles after cleaning. The method has reasonable design, improves the yield of the hydroxyapatite to a great extent, reduces the production cost to a certain extent and meets the market demand.
Description
Technical Field
The invention relates to the field of hydroxyapatite technology, in particular to a hydroxyapatite forming method and application thereof.
Background
Hydroxyapatite (HAP) is the main inorganic component of human and animal bones, it can realize the chemical bond combination with organism tissue on the interface, it has certain solubility in vivo, can release the ion harmless to the organism, can participate in the metabolism in vivo, have stimulating or inducing effects on hyperosteogeny, can promote the defective tissue to repair, reveal the biological activity, at present, hydroxyapatite is applied widely and bone substitute material, plastic and cosmetic surgery, dentistry, chromatography purification, calcium supplement, apply to the tip new material of making and agreeing the tooth or skeleton composition extensively, in addition, because hydroxyapatite has bone inductivity, often apply to the bone tissue regeneration engineering, at present, the yield of hydroxyapatite on the market is less, design a shaping method of hydroxyapatite and application of hydroxyapatite for this.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a hydroxyapatite forming method and application thereof, which greatly improve the yield of hydroxyapatite, reduce the production cost to a certain extent and meet the market demand.
In order to achieve the purpose, the invention adopts the following technical scheme:
a forming method of hydroxyapatite comprises the following steps:
s1: preparing the following raw materials in parts by weight: 15-20 parts of calcium carbonate, 10-15 parts of gypsum, 150-250 parts of purified water, 20-25 parts of calcium chloride, 15-20 parts of milk, 10-15 parts of diammonium phosphate solution and 40-60 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, and respectively marking the interiors of the two reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 10-15min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, respectively marking the stirred reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle after cleaning is finished, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 40-50 ℃, heating for 10-15min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 500-800 r/min, and the rotating and stirring time is 10-15 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 100-120 ℃, carrying out heating reaction for 8-12h, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 10-15min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 30-40 ℃ for 10-15min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the diammonium hydrogen phosphate solution and the concentrated ammonia water, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 200-500 revolutions per minute, and the rotating stirring time is 10-15 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 100-120 ℃, and carrying out heating reaction for 15-20h to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 500-800 r/min, adjusting the temperature of the first stirring reaction kettle to be 120-150 ℃, and heating for 4-8 h;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
Preferably, in S2, the cleaning manner for the reaction cup is flowing water flushing.
Preferably, in S2, the stirring reaction kettle is cleaned by argon replacement reaction.
Compared with the prior art, the invention has the beneficial effects that:
the production method has the advantages that calcium carbonate, gypsum, purified water, calcium chloride, milk, a diammonium hydrogen phosphate solution and concentrated ammonia water are used as main preparation raw materials for processing, the production cost can be reduced to a certain extent, and the product yield can be improved to a great extent by combining reactants using the calcium carbonate, the gypsum and the purified water as raw materials with reactants using the calcium chloride, the milk, the diammonium hydrogen phosphate solution and the concentrated ammonia water as raw materials for processing.
In conclusion, the invention has reasonable design, greatly improves the yield of the hydroxyapatite, reduces the production cost to a certain extent and meets the market demand.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A forming method of hydroxyapatite comprises the following steps:
s1: preparing the following raw materials in parts by weight: 15 parts of calcium carbonate, 10 parts of gypsum, 150 parts of purified water, 20 parts of calcium chloride, 15 parts of milk, 10 parts of diammonium hydrogen phosphate solution and 40 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, washing the reaction cups by flowing water, and respectively marking the reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 10min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, wherein the cleaning mode of the stirring reaction kettles is argon replacement reaction, after cleaning is finished, respectively marking the stirring reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 40 ℃, heating for 10min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the first mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 500 revolutions per minute, and the rotating stirring time is 10 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 100 ℃, carrying out heating reaction for 8 hours, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 10min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 30 ℃ for 10min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 200 revolutions per minute, and the rotating stirring time is 10 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 100 ℃, and carrying out heating reaction for 15 hours to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 500 revolutions per minute, adjusting the temperature of the first stirring reaction kettle to be 120 ℃, and heating for 4 hours;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
Example 2
A forming method of hydroxyapatite comprises the following steps:
s1: preparing the following raw materials in parts by weight: 17 parts of calcium carbonate, 12 parts of gypsum, 180 parts of purified water, 22 parts of calcium chloride, 17 parts of milk, 12 parts of diammonium hydrogen phosphate solution and 45 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, washing the reaction cups by flowing water, and respectively marking the reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 12min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, wherein the cleaning mode of the stirring reaction kettles is argon replacement reaction, after cleaning is finished, respectively marking the stirring reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 44 ℃, heating for 12min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the first mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 600 revolutions per minute, and the rotating stirring time is 12 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 110 ℃, carrying out heating reaction for 9 hours, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 12min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 32 ℃ for 12min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 300 revolutions per minute, and the rotating stirring time is 12 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 110 ℃, and carrying out heating reaction for 17 hours to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 600 revolutions per minute, adjusting the temperature of the first stirring reaction kettle to 130 ℃, and heating for 5 hours;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
Example 3
A forming method of hydroxyapatite comprises the following steps:
s1: preparing the following raw materials in parts by weight: 18 parts of calcium carbonate, 14 parts of gypsum, 220 parts of purified water, 24 parts of calcium chloride, 19 parts of milk, 14 parts of diammonium hydrogen phosphate solution and 55 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, washing the reaction cups by flowing water, and respectively marking the reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 14min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, wherein the cleaning mode of the stirring reaction kettles is argon replacement reaction, after cleaning is finished, respectively marking the stirring reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 48 ℃, heating for 14min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the first mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 700 revolutions per minute, and the rotating and stirring time is 14 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 115 ℃, carrying out heating reaction for 11 hours, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 14min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 38 ℃ for 14min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 400 revolutions per minute, and the rotating stirring time is 14 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 115 ℃, and carrying out heating reaction for 18 hours to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 700 revolutions per minute, adjusting the temperature of the first stirring reaction kettle to be 140 ℃, and heating for 7 hours;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
Example 4
A forming method of hydroxyapatite comprises the following steps:
s1: preparing the following raw materials in parts by weight: 20 parts of calcium carbonate, 15 parts of gypsum, 250 parts of purified water, 25 parts of calcium chloride, 20 parts of milk, 15 parts of diammonium hydrogen phosphate solution and 60 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, washing the reaction cups by flowing water, and respectively marking the reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 15min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, wherein the cleaning mode of the stirring reaction kettles is argon replacement reaction, after cleaning is finished, respectively marking the stirring reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 50 ℃, heating for 15min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the first mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 800 revolutions per minute, and the rotating stirring time is 15 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 120 ℃, carrying out heating reaction for 12 hours, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 15min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 40 ℃ for 15min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 500 revolutions per minute, and the rotating stirring time is 15 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 120 ℃, and carrying out heating reaction for 20 hours to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 800 revolutions per minute, adjusting the temperature of the first stirring reaction kettle to be 150 ℃, and heating for 8 hours;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A forming method of hydroxyapatite is characterized by comprising the following steps:
s1: preparing the following raw materials in parts by weight: 15-20 parts of calcium carbonate, 10-15 parts of gypsum, 150-250 parts of purified water, 20-25 parts of calcium chloride, 15-20 parts of milk, 10-15 parts of diammonium phosphate solution and 40-60 parts of strong ammonia water;
s2: preparing two reaction cups, respectively cleaning the interiors of the two reaction cups, and respectively marking the interiors of the two reaction cups as a first reaction cup and a second reaction cup after cleaning; sequentially putting calcium carbonate and gypsum into a first reaction cup, and then carrying out mixing and stirring work on the interior of the first reaction cup through a stirring rod, wherein the mixing and stirring work time is 10-15min, so as to obtain a first mixture; preparing two stirring reaction kettles, respectively cleaning the interiors of the two stirring reaction kettles, respectively marking the stirred reaction kettles as a first stirring reaction kettle and a second stirring reaction kettle after cleaning is finished, then putting the first mixture into the first stirring reaction kettle, raising the internal temperature of the first stirring reaction kettle to 40-50 ℃, heating for 10-15min, then putting purified water into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle, and stirring and mixing the mixture, wherein the rotating speed of the stirring shaft of the first stirring reaction kettle is 500-800 r/min, and the rotating and stirring time is 10-15 min; after the stirring is finished, adjusting the temperature of the first stirring reaction kettle to 100-120 ℃, carrying out heating reaction for 8-12h, and then keeping for later use;
s3: putting calcium chloride into a second reaction cup, then putting milk into the second reaction cup, and then carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring work time is 10-15min, so as to obtain a mixture II; putting the second mixture into a second stirring reaction kettle, heating the second stirring reaction kettle to 30-40 ℃ for 10-15min, sequentially injecting a diammonium hydrogen phosphate solution and concentrated ammonia water into the second stirring reaction kettle, starting a stirring shaft of the second stirring reaction kettle, and stirring and mixing the diammonium hydrogen phosphate solution and the concentrated ammonia water, wherein the rotating speed of the stirring shaft of the second stirring reaction kettle is 200-500 revolutions per minute, and the rotating stirring time is 10-15 min; after the rotation and the stirring are finished, adjusting the temperature of the second stirring reaction kettle to 100-120 ℃, and carrying out heating reaction for 15-20h to obtain a third mixture;
s4: taking out the mixture III from the second stirring reaction kettle, putting the mixture III into the first stirring reaction kettle, starting a stirring shaft of the first stirring reaction kettle to enable the rotation speed of the stirring shaft to be 500-800 r/min, adjusting the temperature of the first stirring reaction kettle to be 120-150 ℃, and heating for 4-8 h;
s5: closing the first stirring reaction kettle and naturally cooling to obtain a first reactant; and (3) filtering and washing the reactant I, and after washing is finished, carrying out vacuum drying on the reactant I to obtain a reactant II, namely the hydroxyapatite.
2. The method for forming hydroxyapatite according to claim 1, wherein in the step S2, the cleaning means for the reaction cup is flowing water washing.
3. The method for forming hydroxyapatite according to claim 1, wherein in step S2, the cleaning of the stirred tank reactor is argon displacement reaction.
4. Use of hydroxyapatite according to claim 1 in bone tissue regeneration engineering.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116514609A (en) * | 2023-05-11 | 2023-08-01 | 辽宁金秋肥业有限责任公司 | Preparation method of special organic-inorganic compound fertilizer containing high-activity humic acid water rice |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047661A (en) * | 1986-08-07 | 1990-12-12 | 通用食品公司 | The preparation of tricalcium phosphate |
| CN101353371A (en) * | 2007-07-27 | 2009-01-28 | 厦门大学 | H5 subtype avian influenza virus neutralization epitope peptide mimics and uses thereof |
| CN101491690A (en) * | 2009-02-16 | 2009-07-29 | 重庆大学 | Preparation method of nano-micron hydroxylapatite powder |
| CN102649818A (en) * | 2011-02-25 | 2012-08-29 | 厦门大学 | CD4 protein-resistant monoclonal antibody and active fragment and application thereof |
| CN110357056A (en) * | 2019-06-28 | 2019-10-22 | 黄山学院 | A kind of preparation method of hydroxyapatite |
-
2020
- 2020-11-23 CN CN202011321184.3A patent/CN112320779A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047661A (en) * | 1986-08-07 | 1990-12-12 | 通用食品公司 | The preparation of tricalcium phosphate |
| CN101353371A (en) * | 2007-07-27 | 2009-01-28 | 厦门大学 | H5 subtype avian influenza virus neutralization epitope peptide mimics and uses thereof |
| CN101491690A (en) * | 2009-02-16 | 2009-07-29 | 重庆大学 | Preparation method of nano-micron hydroxylapatite powder |
| CN102649818A (en) * | 2011-02-25 | 2012-08-29 | 厦门大学 | CD4 protein-resistant monoclonal antibody and active fragment and application thereof |
| CN110357056A (en) * | 2019-06-28 | 2019-10-22 | 黄山学院 | A kind of preparation method of hydroxyapatite |
Non-Patent Citations (2)
| Title |
|---|
| 王润南等: "贝壳粉制备球形羟基磷灰石", 《化工时刊》 * |
| 石维焕等: "鱼鳞利用的研究进展", 《福建水产》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116514609A (en) * | 2023-05-11 | 2023-08-01 | 辽宁金秋肥业有限责任公司 | Preparation method of special organic-inorganic compound fertilizer containing high-activity humic acid water rice |
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