CN102885698B - A kind of ultra micro hydrocolloid powder possessing core, shell structure and its production and use - Google Patents
A kind of ultra micro hydrocolloid powder possessing core, shell structure and its production and use Download PDFInfo
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- CN102885698B CN102885698B CN201210400375.8A CN201210400375A CN102885698B CN 102885698 B CN102885698 B CN 102885698B CN 201210400375 A CN201210400375 A CN 201210400375A CN 102885698 B CN102885698 B CN 102885698B
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- 239000000843 powder Substances 0.000 title claims abstract description 98
- 239000000416 hydrocolloid Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title description 5
- 239000000839 emulsion Substances 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 38
- 239000000084 colloidal system Substances 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 10
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 33
- 238000013019 agitation Methods 0.000 claims description 24
- 239000011521 glass Substances 0.000 claims description 20
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000661 sodium alginate Substances 0.000 claims description 14
- 235000010413 sodium alginate Nutrition 0.000 claims description 14
- 229940005550 sodium alginate Drugs 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical group O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 229920000159 gelatin Polymers 0.000 claims description 8
- 235000019322 gelatine Nutrition 0.000 claims description 8
- 238000003828 vacuum filtration Methods 0.000 claims description 8
- 150000001718 carbodiimides Chemical class 0.000 claims description 6
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims description 6
- 239000001828 Gelatine Substances 0.000 claims description 5
- AZKVWQKMDGGDSV-BCMRRPTOSA-N Genipin Chemical compound COC(=O)C1=CO[C@@H](O)[C@@H]2C(CO)=CC[C@H]12 AZKVWQKMDGGDSV-BCMRRPTOSA-N 0.000 claims description 5
- 241001597008 Nomeidae Species 0.000 claims description 5
- AZKVWQKMDGGDSV-UHFFFAOYSA-N genipin Natural products COC(=O)C1=COC(O)C2C(CO)=CCC12 AZKVWQKMDGGDSV-UHFFFAOYSA-N 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 5
- 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 claims description 5
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 4
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000001506 calcium phosphate Substances 0.000 claims description 4
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 229910000389 calcium phosphate Inorganic materials 0.000 claims 1
- 235000011010 calcium phosphates Nutrition 0.000 claims 1
- 239000004531 microgranule Substances 0.000 abstract description 17
- 239000000654 additive Substances 0.000 abstract description 13
- 230000000996 additive effect Effects 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 10
- 230000006378 damage Effects 0.000 abstract description 4
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000011806 microball Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- 229940034610 toothpaste Drugs 0.000 description 8
- 239000000606 toothpaste Substances 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 6
- 210000005239 tubule Anatomy 0.000 description 6
- 210000003298 dental enamel Anatomy 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000000586 desensitisation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 210000004268 dentin Anatomy 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229940078499 tricalcium phosphate Drugs 0.000 description 3
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 3
- 235000019731 tricalcium phosphate Nutrition 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 235000010443 alginic acid Nutrition 0.000 description 2
- 229960001126 alginic acid Drugs 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 229920000615 alginic acid Polymers 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 208000002925 dental caries Diseases 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- SYUXAJSOZXEFPP-UHFFFAOYSA-N glutin Natural products COc1c(O)cc2OC(=CC(=O)c2c1O)c3ccccc3OC4OC(CO)C(O)C(O)C4O SYUXAJSOZXEFPP-UHFFFAOYSA-N 0.000 description 2
- 239000013521 mastic Substances 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007634 remodeling Methods 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229940090898 Desensitizer Drugs 0.000 description 1
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 description 1
- 108090000723 Insulin-Like Growth Factor I Proteins 0.000 description 1
- 206010022998 Irritability Diseases 0.000 description 1
- 241001354782 Nitor Species 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical group [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 102000013275 Somatomedins Human genes 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000008468 bone growth Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
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- -1 phosphonium ion Chemical class 0.000 description 1
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Landscapes
- Cosmetics (AREA)
Abstract
The invention discloses a kind of ultra micro hydrocolloid powder possessing core, shell structure, the particle diameter of described ultra micro microgranule is 0.01 10 μm, and described ultra micro microgranule includes that kernel and spherical housing, described kernel are inorganic substances, described spherical housing is colloid, and described spherical housing passes through cross-linking agent curing molding.The invention also discloses the preparation method of a kind of ultra micro hydrocolloid powder, comprise the following steps: prepare ultra micro inanimate matter powder；Add water and prepare the ultra micro suspended aqueous solution of inanimate matter powder；Prepare colloid aqueous solution；It is mixed with colloid inanimate matter emulsion；Add cross-linking agent and prepare crosslinked gel inanimate matter emulsion；Add methanol or ethanol chromatography ultra micro colloid micro ball shape particle；Cyclic washing final vacuum sucking filtration, dried prepared ultra micro hydrocolloid powder.The invention also discloses the purposes of a kind of ultra micro hydrocolloid powder, it is used as oral preparation additive.The ultra micro hydrocolloid powder of the present invention has inanimate matter effect, simultaneously because its shell is spherical, so contact organism will not be caused damage.
Description
Technical field
The present invention relates to a kind of ultra-micro powder and its production and use, particularly relate to a kind of possess core, shell structure
Ultra micro hydrocolloid powder and its production and use.
Background technology
Ultra-micro powder is usually used in the additive of some preparations, is jointly made as liquid or mastic.At these liquid or mastic
It is applied to organism local time, owing to the ultra micro particulate form of ultra-micro powder is irregular, has corner angle, it is possible that can be to organism
Cause damage, thus cause new problem to produce so that it is application is severely limited.Have as a example by tooth paste product below
Body illustrates:
The China's epidemiological investigation data that can announce of stomatology shows: China 20-60 year adult in have
The people of 29.7% can be perplexed by dentine hypersensitivity every day.This mean that China almost 1/3rd crowd all exist
Bear tooth and meet the pain that physics, the chemical machinery sexual stimulus such as hot and cold, sour, sweet bring.
The root that dentin hypersensitiveness patient is worried comes from traditional Therapeutic Method imperfection.The biography of dentin hypersensitiveness at present
Rule to treat and carry out substantially about two aspects: one, the permeability of change dentinal tubule: the method for Clinical practice mainly has sharp
Light treatment and chemical agent therapy, curative effect all less stables, and all tooth itself and periodontal tissue can be caused chemical
Damage；Two, reduce Intradental nerve irritability: mainly utilize the composition of potassium ion, reduce nerve conduction current potential, benumb pain,
Mitigation symptoms.Mostly desensitizing toothpaste the method, can appropriateness alleviating pain, but still can continuous recurrent exerbation, it is impossible to play root
This therapeutic effect.
For professional treatment dental hypersensitiveness, famous American dental pulp disease expert Grossman proposes six standards: 1,
Non-stimulated to dental pulp；Relatively without pain when 2, using；3, easily operate；4, effect is rapidly；5, effect stability；6, tooth is not made
Color.So far to this end, still do not have a kind of desensitizer to comply fully with above-mentioned standard.Clinically in the urgent need to the appearance of new material.
For a long time, glass is considered as a kind of inert material, is mainly used as container, such as laboratory device in terms of medical science
Ware, test tube etc..But, research shows: glass can not only participate in hemagglutination, and can accelerate blood coagulation, and this illustrates glass surface
It not inert, but activity.Along with vagcor progress of research, people obtain micropore glass, its specific surface area
The imagination beyond people big with activity, so that glass has obtained new use biomedical in terms of Biochemical Engineering
On the way.
1971, professor Hench found Na2O—CaO—SiO2—P2O5The glass material of system is implanted in organism,
Component in material can be intercoursed with the component in organism or react, and ultimately forms the thing compatible with organism itself
Matter, constitutes newborn skeleton or a part for tooth.Thus, draw the concept of bioactivity glass, open glass for curing
Learn important one page of clinical research.Research also finds, bioactivity glass not only has promotion bone growth and remineralization is made
With, but also there is the inhibitory action of Oral Bacteria, this brings a brand-new theory to clinical oral treatment again.
But, a dentin treatment often long-term lasting process, micro-in common bioactivity glass powder
Grain is corner angle inanimate matter granules clearly demarcated, scleroid, when treating in being directly appended to the preparations such as desensitizing toothpaste, does not allows
Easily fully firmly it is filled in the dentinal tubule exposed to the open air；Even if dentinal tubule can be filled and mineralising reparation, but brush
Friction repeatedly during tooth, sharp bioactive glass particle frequently can lead to part dental enamel table surface wear, thus brings new
Oral problem.Therefore, how bioactivity glass more effectively can be used for dental care is a problem merited attention.
Presently disclosed document yet there are no relevant report, does not more solve the practical application example of this problem.
Summary of the invention
The purpose of the present invention is that provides a kind of ultra micro colloid powder possessing core, shell structure to solve the problems referred to above
End and its production and use.
In order to achieve the above object, present invention employs techniques below scheme:
The ultra micro hydrocolloid powder possessing core, shell structure of the present invention, is made up of ultra micro microgranule, the grain of described ultra micro microgranule
Footpath is 0.01-10 μm, and described ultra micro microgranule includes that kernel and spherical housing, described kernel are inorganic substances, described spherical housing
For colloid, described spherical housing passes through cross-linking agent curing molding.
Above-mentioned ultra micro hydrocolloid powder being applied to biological preparation additive, becomes sticky when meeting water, its ultra micro microgranule is easier to jail
Admittedly clog in the gap of application, it is ensured that the abundant mineralising repair of ultra micro hydrocolloid powder；It addition, round and smooth table
Face the most farthest reduces the infringement that application is caused in friction process by the ultra micro microgranule of ultra micro hydrocolloid powder.
Specifically, during described kernel is bioactivity glass, hydroxyapatite, calcium bicarbonate, calcium carbonate and tricalcium phosphate
Any one；Described spherical housing is any in sodium alginate, sodium alginate derivant, gelatin and gelatine derivative
Kind；Described cross-linking agent is in glutaraldehyde, genipin, polypropylene glycol glycidyl ether, maleic anhydride and carbodiimides
Any.
As preferably, the particle diameter of described ultra micro microgranule is 0.1-2 μm；Most preferably 0.5-1 μm.
The preparation method of ultra micro hydrocolloid powder of the present invention, comprises the following steps:
(1) inorganic substances by 0.1～50 weight portions are levigate, and prepared mean diameter is the ultra micro inanimate matter of 0.1～1.8 μm
Powder；
(2) water to 10～200 weight portions carries out the high-speed ultrasonic stirring of 1000～7000r/min, supersonic vibration frequency
Being 22～35KHz, the ultrasonic intermittent time is 0.5～15min, and the ultra micro inanimate matter powder that step (1) prepares is uniformly added into water
In solution, obtain the ultra micro suspended aqueous solution of inanimate matter powder；
(3) colloid of 10～200 weight portions is joined in the water of 30～1000 weight portions, by 1000～5000r/
The high-speed ultrasonic stirring of min, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is 0.5～15min, during ultrasonic agitation
Between be 0.5～10h, prepare colloid aqueous solution；
(4) colloid aqueous solution to 100～1000 weight portions that step (3) prepares carries out the height of 1000～7000r/min
Speed ultrasonic agitation, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is 0.5～15min, and step (2) prepared is super
Micro-suspended aqueous solution of inanimate matter powder at the uniform velocity added in 2～30 minutes, adjust mixed solution pH value in the range of 4～7.5,
The colloid being uniformly mixed-inanimate matter emulsion；
(5) taking cross-linking agent, described cross-linking agent accounts for the 0.05 of the gross mass of colloid-inanimate matter emulsion that step (4) prepares
～12%, described cross-linking agent is at the uniform velocity joined in described colloid-inanimate matter emulsion, keep 2000～8000r/min ultrasonic
Mixing speed, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is 0.5～15min, is 10nm～400nm at wavelength
Ultraviolet light irradiate lower reaction 5～60h, the crosslinked gel being uniformly mixed-inanimate matter emulsion；
(6) methanol of 500～5000 weight portions or ethanol are carried out the high-speed ultrasonic stirring of 1000～5000r/min, super
Sound vibration frequency is 20～30KHz, and the ultrasonic intermittent time is 1～10min, crosslinked gel step (5) prepared-inanimate matter breast
Turbid liquid at the uniform velocity adds, and chromatographs excess of export idiozome particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 6.5-7.5, through vacuum filtration, will
Ultra micro colloidal particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.01-10 μm.
As preferably: in described step (1), the weight portion of described inorganic substances is 10～30, described ultra micro inanimate matter powder
The mean diameter at end is 0.3～1.2 μm；The weight portion of described water is 50～100, and the speed of described high-speed ultrasonic stirring is 3000
～5000r/min, described supersonic vibration frequency is 25～30KHz, and the described ultrasonic intermittent time is 5～10min；Described step
(3) in, the weight portion of described colloid is 50～150, and the weight portion of described water is 200～500, the speed of described high-speed ultrasonic stirring
Degree is 2000～4000r/min, and described supersonic vibration frequency is 25～30KHz, and the described ultrasonic intermittent time is 5～10min, institute
Stating the ultrasonic agitation time is 3～8h；In described step (4), the weight portion of described colloid aqueous solution is 500～700, described high speed
The speed of ultrasonic agitation is 3000～5000r/min, and described frequency of vibration is 25～30KHz, the described intermittent time be 5～
10min, the described ultra micro suspended aqueous solution of inanimate matter powder at the uniform velocity added in 10～20 minutes, adjusted described mixed solution pH value
In the range of 6～7.5；In described step (5), described cross-linking agent account for the gross mass of described colloid-inanimate matter emulsion 3～
6%, described ultrasonic agitation speed is 4000～6000r/min, and described supersonic vibration frequency is 25～30KHz, described ultrasonic interval
Time is 5～10min, and the wavelength of described ultraviolet light is 100nm～200nm, and the described response time is 20～30h；Described step
(6) in, the weight portion of described methanol or ethanol is 2000～4000, and the speed of described high-speed ultrasonic stirring is 2000～4000r/
Min, described frequency of vibration is 23～26KHz, and the described intermittent time is 3～6min；In described step (7), described pH value is 7,
The ultra micro diameter of particle of described ultra micro hydrocolloid powder is 0.01-10 μm.
The purposes of ultra micro hydrocolloid powder of the present invention, it is used as oral preparation additive；It is particularly suitable for adding as toothpaste
Add agent.
The beneficial effects of the present invention is:
Ultra micro hydrocolloid powder of the present invention being applied to biological preparation additive, becomes sticky when meeting water, its ultra micro microgranule is more
Easily clog securely in the gap of application, it is ensured that the abundant mineralising repair of ultra micro hydrocolloid powder；It addition, circle
Sliding surface the most farthest reduces what application was caused in friction process by the ultra micro microgranule of ultra micro hydrocolloid powder
Infringement.
Ultra micro hydrocolloid powder of the present invention is used as toothpaste additive, and the colloidal substance of its ultra micro microparticle surfaces is met water and is become
Viscous, it is easier to firmly to clog dentinal tubule, it is ensured that the abundant mineralising reparation of inanimate matter such as bioactivity glass；The opposing party
Face, round and smooth surface the most farthest reduces the infringement that enamel is caused in friction process by ultra micro microgranule.
Ultra micro hydrocolloid powder of the present invention also has desensitizing dental effect that common inorganic material is incomparable.First
First, when hydrocolloid powder is entering oral cavity, when running into water or saliva, absorbing water rapidly, discharge sodium ion, pH is increased to 8.5, in office
Portion forms weakly alkaline environment, and weakly alkaline environment is just beneficial to cemental reconstruction；Then, inanimate matter such as bioactivity glass is released
Putting calcium, phosphonium ion, these are the necessary raw materials of bony remodeling, SiO therein2, due to electronegative, absorption can be got started
Structoure of the human body matrix such as somatomedin, collagen protein etc. needed for tissue regeneration, and network structure can be built, trouble can be made
Sick position forms hydroxyapatite layer (HA), similar to dentium nitor face chemical composition structure；Block so rapidly and cover exposure
Dentinal tubule, makes enamel reach the effect of remineralization, strengthens desensitization.
The sodium of ultra micro hydrocolloid powder of the present invention release, calcium ion can change the water balance inside and outside antibacterial, cause thin
Bacterium dehydration death, plays obvious bactericidal action, so serves beyond thought to diseases such as clinical gingivitis, periodontitis
Effect.
Owing to the reparation of the inanimate matter such as bioactivity glass of ultra micro hydrocolloid powder of the present invention is that a kind of physiological is repaiied
Multiple rather than simple blocking-up and paralysis；Degree of depth remineralization repairing dental enamel defect and dentinal tubule inherently improve
The state of tooth, the features such as the floride-free formula of safety, easy to use simultaneously, Anti-dental injury gum, substantially meet oral cavity expert
Six standards that Grossman proposes.
It addition, ultra micro hydrocolloid powder of the present invention can be widely applied on the remodeling of other dentifrice abrasives, sending out
While waving desensitization effect of brilliance, efficiently avoid again common inorganic matter additive during life-time service to enamel
The new abrasion that surface is caused, and beneficially preparation of industrialization.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described in detail:
Embodiment 1:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) bioactivity glass of 0.1 weight portion is levigate by ball milling, then sieve, prepared mean diameter be 0.3～
The ultra micro inanimate matter powder of 0.8 μm；
(2) water to 10 weight portions carries out the high-speed ultrasonic stirring of 1000r/min, and supersonic vibration frequency is 22KHz, ultrasonic
Intermittent time is 0.5min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inanimate matter
The suspended aqueous solution of powder；
(3) sodium alginate of 10 weight portions is joined in the water of 30 weight portions, stirred by the high-speed ultrasonic of 1000r/min
Mixing, supersonic vibration frequency is 22KHz, and the ultrasonic intermittent time is 0.5min, and the ultrasonic agitation time is 0.5h, prepares colloid water-soluble
Liquid；
(4) colloid aqueous solution to 100 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 1000r/min, super
Sound vibration frequency is 22KHz, and the ultrasonic intermittent time is 0.5min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 2 minutes, and adjusting mixed solution pH value is 4, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking glutaraldehyde, glutaraldehyde accounts for the 0.05% of the gross mass of colloid-inanimate matter emulsion that step (4) prepares, will
Glutaraldehyde at the uniform velocity joins in described colloid-inanimate matter emulsion, keeps the ultrasonic agitation speed of 2000r/min, supersonic vibration
Frequency is 22KHz, and the ultrasonic intermittent time is 0.5min, reacts 5h under the ultraviolet light that wavelength is 10nm irradiates, and obtains mixing all
Even crosslinked gel-inanimate matter emulsion；
(6) methanol to 500 weight portions carries out the high-speed ultrasonic stirring of 1000r/min, and supersonic vibration frequency is 20KHz,
The ultrasonic intermittent time is 1min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out ultra micro glue
Body particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 6.5, through vacuum filtration, by ultra micro
Colloidal particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes bioactivity glass kernel and alginic acid
Sodium spherical housing, sodium alginate spherical housing passes through glutaraldehyde curing molding.This ultra micro hydrocolloid powder is suitable for be prevented as tooth
Dental caries desensitization formulation additives.
Embodiment 2:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) hydroxyapatite of 5 weight portions is levigate by ball milling, then sieve, prepared mean diameter is 0.3～0.8 μm
Ultra micro inanimate matter powder；
(2) water to 30 weight portions carries out the high-speed ultrasonic stirring of 2000r/min, and supersonic vibration frequency is 23KHz, super
The sound intermittent time is 3min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inanimate matter
The suspended aqueous solution of powder；
(3) the sodium alginate derivant of 30 weight portions is joined in the water of 80 weight portions, by the height of 1500r/min
Speed ultrasonic agitation, supersonic vibration frequency is 23KHz, and the ultrasonic intermittent time is 3min, and the ultrasonic agitation time is 2h, prepares colloid water
Solution；
(4) colloid aqueous solution to 200 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 2000r/min,
Supersonic vibration frequency is 25KHz, and the ultrasonic intermittent time is 3min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 5 minutes, and adjusting mixed solution pH value is 5, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking genipin, genipin accounts for the 1% of the gross mass of colloid-inanimate matter emulsion that step (4) prepares, by capital
The even speed of Buddhist nun joins in described colloid-inanimate matter emulsion, keeps the ultrasonic agitation speed of 3000r/min, supersonic vibration frequency
Rate is 23KHz, and the ultrasonic intermittent time is 3min, reacts 10h, be uniformly mixed under the ultraviolet light that wavelength is 50nm irradiates
Crosslinked gel-inanimate matter emulsion；
(6) methanol to 1000 weight portions carries out the high-speed ultrasonic stirring of 1500r/min, and supersonic vibration frequency is
22KHz, the ultrasonic intermittent time is 2min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out
Ultra micro colloidal particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 7, through vacuum filtration, by ultra micro glue
Body particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes hydroxyapatite kernel and sodium alginate
Derivant spherical housing, sodium alginate derivant spherical housing passes through genipin curing molding.This ultra micro hydrocolloid powder is suitable for
As desensitizing toothpaste additive.
Embodiment 3:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) calcium bicarbonate of 10 weight portions is levigate by ball milling, then sieve, prepared mean diameter is 0.3～0.8 μm
Ultra micro inanimate matter powder；
(2) water to 50 weight portions carries out the high-speed ultrasonic stirring of 3000r/min, and supersonic vibration frequency is 25KHz, super
The sound intermittent time is 5min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inanimate matter
The suspended aqueous solution of powder；
(3) gelatin of 50 weight portions is joined in the water of 200 weight portions, stirred by the high-speed ultrasonic of 2000r/min
Mixing, supersonic vibration frequency is 25KHz, and the ultrasonic intermittent time is 5min, and the ultrasonic agitation time is 5h, prepares colloid aqueous solution；
(4) colloid aqueous solution to 500 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 3000r/min,
Supersonic vibration frequency is 25KHz, and the ultrasonic intermittent time is 5min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 10 minutes, and adjusting mixed solution pH value is 6, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking polypropylene glycol glycidyl ether, polypropylene glycol glycidyl ether accounts for colloid-inanimate matter that step (4) prepares
The 3% of the gross mass of emulsion, at the uniform velocity joins polypropylene glycol glycidyl ether in described colloid-inanimate matter emulsion, keeps
The ultrasonic agitation speed of 4000r/min, supersonic vibration frequency is 25KHz, and the ultrasonic intermittent time is 5min, is 100nm at wavelength
Ultraviolet light irradiate under react 20h, the crosslinked gel being uniformly mixed-inanimate matter emulsion；
(6) ethanol to 2000 weight portions carries out the high-speed ultrasonic stirring of 2000r/min, and supersonic vibration frequency is
23KHz, the ultrasonic intermittent time is 3min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out
Ultra micro colloidal particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 7, through vacuum filtration, by ultra micro glue
Body particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes outside calcium bicarbonate kernel and glutin spherical
Shell, glutin spherical shell passes through polypropylene glycol glycidyl ether curing molding.This ultra micro hydrocolloid powder is suitable for and is used as common tooth
Paste additive.
Embodiment 4:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) calcium carbonate of 30 weight portions is levigate by ball milling, then sieve, prepared mean diameter is 0.3～0.8 μm
Ultra micro inanimate matter powder；
(2) water to 100 weight portions carries out the high-speed ultrasonic stirring of 5000r/min, and supersonic vibration frequency is 30KHz, super
The sound intermittent time is 10min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inorganic
The suspended aqueous solution of matter powder；
(3) gelatine derivative of 150 weight portions is joined in the water of 500 weight portions, by the high speed of 4000r/min
Ultrasonic agitation, supersonic vibration frequency is 30KHz, and the ultrasonic intermittent time is 10min, and the ultrasonic agitation time is 8h, prepares colloid water
Solution；
(4) colloid aqueous solution to 700 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 5000r/min,
Supersonic vibration frequency is 30KHz, and the ultrasonic intermittent time is 10min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 20 minutes, and adjusting mixed solution pH value is 7, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking maleic anhydride, maleic anhydride accounts for total matter of colloid-inanimate matter emulsion that step (4) prepares
The 6% of amount, at the uniform velocity joins in described colloid-inanimate matter emulsion by maleic anhydride, keeps the ultrasonic of 6000r/min to stir
Mixing speed, supersonic vibration frequency is 30KHz, and the ultrasonic intermittent time is 10min, anti-under the ultraviolet light that wavelength is 200nm irradiates
Answer 30h, the crosslinked gel being uniformly mixed-inanimate matter emulsion；
(6) ethanol to 4000 weight portions carries out the high-speed ultrasonic stirring of 4000r/min, and supersonic vibration frequency is
26KHz, the ultrasonic intermittent time is 6min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out
Ultra micro colloidal particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 7.2, through vacuum filtration, by ultra micro
Colloidal particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes calcium carbonate kernel and gelatine derivative ball
Shape shell, gelatine derivative spherical housing passes through maleic anhydride curing molding.This ultra micro hydrocolloid powder is suitable for as general
Logical toothpaste additive.
Embodiment 5:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) tricalcium phosphate of 50 weight portions is levigate by ball milling, then sieve, prepared mean diameter is 0.3～0.8 μm
Ultra micro inanimate matter powder；
(2) water to 200 weight portions carries out the high-speed ultrasonic stirring of 7000r/min, and supersonic vibration frequency is 35KHz, super
The sound intermittent time is 15min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inorganic
The suspended aqueous solution of matter powder；
(3) sodium alginate of 200 weight portions is joined in the water of 1000 weight portions, surpassed by the high speed of 5000r/min
Sound stirs, and supersonic vibration frequency is 35KHz, and the ultrasonic intermittent time is 15min, and the ultrasonic agitation time is 10h, prepares colloid water-soluble
Liquid；
(4) colloid aqueous solution to 1000 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 7000r/min,
Supersonic vibration frequency is 35KHz, and the ultrasonic intermittent time is 15min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 30 minutes, and adjusting mixed solution pH value is 7.5, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking carbodiimides, carbodiimides accounts for the gross mass of colloid-inanimate matter emulsion that step (4) prepares
12%, carbodiimides is at the uniform velocity joined in described colloid-inanimate matter emulsion, keep the ultrasonic agitation speed of 8000r/min
Degree, supersonic vibration frequency is 35KHz, and the ultrasonic intermittent time is 15min, reacts under the ultraviolet light that wavelength is 400nm irradiates
60h, the crosslinked gel being uniformly mixed-inanimate matter emulsion；
(6) methanol to 5000 weight portions carries out the high-speed ultrasonic stirring of 5000r/min, and supersonic vibration frequency is
30KHz, the ultrasonic intermittent time is 10min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out
Ultra micro colloidal particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 7.5, through vacuum filtration, by ultra micro
Colloidal particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes tricalcium phosphate kernel and sodium alginate ball
Shape shell, sodium alginate spherical housing passes through carbodiimides curing molding.This ultra micro hydrocolloid powder is suitable for and is used as common tooth
Paste additive.
Embodiment 6:
Prepare ultra micro hydrocolloid powder according to the following steps:
(1) bioactivity glass of 40 weight portions is levigate by ball milling, then sieve, prepared mean diameter be 0.3～
The ultra micro inanimate matter powder of 0.8 μm；
(2) water to 150 weight portions carries out the high-speed ultrasonic stirring of 5000r/min, and supersonic vibration frequency is 30KHz, super
The sound intermittent time is 12min, is uniformly added in aqueous solution by the ultra micro inanimate matter powder that step (1) prepares, obtains ultra micro inorganic
The suspended aqueous solution of matter powder；
(3) sodium alginate of 180 weight portions is joined in the water of 800 weight portions, surpassed by the high speed of 3000r/min
Sound stirs, and supersonic vibration frequency is 30KHz, and the ultrasonic intermittent time is 12min, and the ultrasonic agitation time is 8h, prepares colloid water-soluble
Liquid；
(4) colloid aqueous solution to 800 weight portions that step (3) prepares carries out the high-speed ultrasonic stirring of 6000r/min,
Supersonic vibration frequency is 30KHz, and the ultrasonic intermittent time is 12min, and ultra micro inanimate matter powder step (2) prepared is suspended water-soluble
Liquid at the uniform velocity added in 25 minutes, and adjusting mixed solution pH value is 7, the colloid being uniformly mixed-inanimate matter emulsion；
(5) taking glutaraldehyde, glutaraldehyde accounts for the 8% of the gross mass of colloid-inanimate matter emulsion that step (4) prepares, by penta
Dialdehyde at the uniform velocity joins in described colloid-inanimate matter emulsion, keeps the ultrasonic agitation speed of 6000r/min, supersonic vibration frequency
Rate is 30KHz, and the ultrasonic intermittent time is 12min, reacts 50h, be uniformly mixed under the ultraviolet light that wavelength is 300nm irradiates
Crosslinked gel-inanimate matter emulsion；
(6) ethanol to 4000 weight portions carries out the high-speed ultrasonic stirring of 4000r/min, and supersonic vibration frequency is
28KHz, the ultrasonic intermittent time is 8min, is at the uniform velocity added by crosslinked gel-inanimate matter emulsion that step (5) prepares, chromatographs out
Ultra micro colloidal particle；
(7) the ultra micro colloidal particle that cyclic washing step (6) prepares, after pH value is 7, through vacuum filtration, by ultra micro glue
Body particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.5-1 μm.
Ultra micro microgranule through the ultra micro hydrocolloid powder of said method acquisition includes bioactivity glass kernel and alginic acid
Sodium spherical housing, sodium alginate spherical housing passes through glutaraldehyde curing molding.This ultra micro hydrocolloid powder is suitable for be prevented as tooth
Dental caries desensitization formulation additives.
In above-mentioned all embodiments, the weight of each raw material does not provides concrete unit, is because can having according to actual needs many
Plant unit to select, depending on the concrete weight demand according to the ultra micro hydrocolloid powder needed for producing.
Claims (2)
1. the preparation method of the ultra micro hydrocolloid powder possessing core, shell structure, it is characterised in that: comprise the following steps:
(1), using levigate for the inorganic substances as kernel of 0.1～50 weight portions, prepared mean diameter is 0.1～1.8 μm
Ultra micro inanimate matter powder；(2), the water to 10～200 weight portions carries out the high speed of 1000～7000r/min
Ultrasonic agitation, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is 0.5～15min, step (1) is prepared
Ultra micro inanimate matter powder be uniformly added in aqueous solution, obtain the ultra micro suspended aqueous solution of inanimate matter powder；(3), by 10～
The colloid of 200 weight portions joins in the water of 30～1000 weight portions, by the high speed of 1000～5000r/min
Ultrasonic agitation, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is 0.5～15min, the ultrasonic agitation time
It is 0.5～10h, prepares colloid aqueous solution；(4), to step (3) prepare 100～1000 weight portions as ball
The colloid aqueous solution of shape shell carry out 1000～7000r/min high-speed ultrasonic stirring, supersonic vibration frequency be 22～
35KHz, the ultrasonic intermittent time is 0.5～15min, and the ultra micro suspended aqueous solution of inanimate matter powder step (2) prepared is 2
～at the uniform velocity add in 30 minutes, adjust mixed solution pH value in the range of 4～7.5, the glue being uniformly mixed
Body-inanimate matter emulsion；(5), taking cross-linking agent, described cross-linking agent accounts for colloid-inanimate matter emulsion that step (4) prepares
Gross mass 0.05～12%, described cross-linking agent is at the uniform velocity joined in described colloid-inanimate matter emulsion, keep
The ultrasonic agitation speed of 2000～8000r/min, supersonic vibration frequency is 22～35KHz, and the ultrasonic intermittent time is
0.5～15min, under the ultraviolet light that wavelength is 10nm～400nm irradiates, react 5～60h, be uniformly mixed
Crosslinked gel-inanimate matter emulsion；(6), the methanol of 500～5000 weight portions or ethanol are carried out 1000～
5000r/min high-speed ultrasonic stirring, supersonic vibration frequency is 20～30KHz, the ultrasonic intermittent time be 1～
10min, at the uniform velocity adds crosslinked gel-inanimate matter emulsion that step (5) prepares, and chromatographs excess of export idiozome particle；
(7), cyclic washing step (6) prepare ultra micro colloidal particle, after pH value is 6.5-7.5, through vacuum filtration, by ultra micro
Colloidal particle lyophilization, prepared particle diameter is the ultra micro hydrocolloid powder of 0.01-10 μm；Described ultra micro hydrocolloid powder includes kernel
And spherical housing, described kernel is any in bioactivation glass, hydroxyapatite, calcium bicarbonate, calcium carbonate and calcium phosphate
One, described spherical housing is any one of sodium alginate, sodium alginate derivant, gelatin and gelatine derivative, described
Spherical housing passes through cross-linking agent curing molding；Described cross-linking agent is glutaraldehyde, genipin, polypropylene glycol glycidyl ether, suitable fourth
Any one of enedioic acid acid anhydride and carbodiimides.
The preparation method of a kind of ultra micro hydrocolloid powder possessing core, shell structure the most according to claim 1, its feature exists
In: in described step (1), the weight portion of described inorganic substances is 10～30, and the mean diameter of described ultra micro inanimate matter powder is
0.3～1.2 μm；The weight portion of described water is 50～100, and the speed of described high-speed ultrasonic stirring is 3000～5000r/
Min, described supersonic vibration frequency is 25～30KHz, and the described ultrasonic intermittent time is 5～10min；Described step (3)
In, the weight portion of described colloid is 50～150, and the weight portion of described water is 200～500, and described high-speed ultrasonic stirs
Speed be 2000～4000r/min, described supersonic vibration frequency is 25～30KHz, and the described ultrasonic intermittent time is
5～10min, the described ultrasonic agitation time is 3～8h；In described step (4), the weight portion of described colloid aqueous solution is
500～700, described high-speed ultrasonic stirring speed be 3000～5000r/ min, described frequency of vibration be 25～
30KHz, the described intermittent time is 5～10min, and the described ultra micro suspended aqueous solution of inanimate matter powder was at 10～20 minutes
The most at the uniform velocity add, adjust described mixed solution pH value in the range of 6～7.5；In described step (5), described crosslinking
Agent accounts for the 3～6% of the gross mass of described colloid-inanimate matter emulsion, described ultrasonic agitation speed be 4000～
6000r/min, supersonic vibration frequency is 25～30KHz, and the ultrasonic intermittent time is 5～10min, described ultraviolet light
Wavelength is 100nm～200nm, and the described response time is 20～30h；In described step (6), described methanol or ethanol
Weight portion be 2000～4000, described high-speed ultrasonic stirring speed be 2000～4000r/min, described vibration frequency
Rate is 23～26KHz, and the described intermittent time is 3～6min；In described step (7), described pH value is 7, described
The ultra micro diameter of particle of ultra micro hydrocolloid powder is 0.01-10 μm.
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