CN108341607A - A kind of silica modified magnesia and its preparation method and application - Google Patents
A kind of silica modified magnesia and its preparation method and application Download PDFInfo
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- CN108341607A CN108341607A CN201810205456.XA CN201810205456A CN108341607A CN 108341607 A CN108341607 A CN 108341607A CN 201810205456 A CN201810205456 A CN 201810205456A CN 108341607 A CN108341607 A CN 108341607A
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- magnesia
- silica modified
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- tetraethyl orthosilicate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0042—Powdery mixtures
-
- 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
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
-
- 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
- A61L27/58—Materials at least partially resorbable by the body
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
- C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00025—Aspects relating to the protection of the health, e.g. materials containing special additives to afford skin protection
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
Abstract
The present invention discloses a kind of preparation method and applications of silica modified magnesia, is mainly used in the bone renovating material using magnesia as raw material, preparation method is：1) by magnesia calcination processing, ball milling obtains magnesium oxide powder after calcining, takes a certain amount of magnesia evenly dispersed in organic solvent, forms magnesia magma；2) tetraethyl orthosilicate solution and catalyst solution are added in the suspension containing magnesia, be stirred to react, wash it is dry after obtain the magnesia that coated with silica is modified.The present invention can regulate and control mgo surface property by the modified oxidized magnesium of coated with silica.When using magnesia as magnesium-based bone cement prepared by raw material, it can need to adjust the cladding degree of magnesia according to clinic to change hardening time, and hydration temperature when bone renovating material solidification can be reduced, it is remarkably improved using magnesia as the performance of the bone renovating material of raw material.
Description
Technical field
The present invention relates to field of inorganic material preparing technology, it is related to a kind of preparation method of silica modified magnesia and its answers
With being mainly used in bio-medical material using magnesia as the bone renovating material of raw material.
Technical background
Using magnesia as the bone renovating material of raw material in bio-medical material, there is fast solidifying, high early strong characteristic, it can be
Voluntarily cured under human physiological environment, the interface cohesion of high intensity can be formed with bone tissue, hydrated product is phosphoric acid salt
Biological ore, hydrated product have good biocompatibility, have no toxic side effect.MgO activity is high, and reaction speed is fast, heat release
Amount is big, these heats further accelerate the reaction speed of system, lead to rate of set quickly, and solidifying characteristic seriously affects soon
The popularization of magnesium phosphate cement and the application range for limiting it are lived frequently with high temperature sintering to lower its reaction in use
Property, or slow down the reaction process of magnesia by adding retarder, chelating agent.Make by high temperature sintering and extension sintering time
Magnesia grain size increases, and a large amount of magnesia is remained after reaction, can be generated to the fluid environment of human body during material degradation
Interference, side effect are apparent.
Invention content
The technical problem to be solved in the present invention is to overcome the deficiencies of existing technologies, and provides a kind of silica modified oxidation
The preparation method and applications of magnesium reach using magnesia as the controllability of the bone renovating material curing reaction of raw material, and are dropping
Silicon ion is discharged in solution preocess.
In order to solve the above technical problems, the present invention uses following technical proposals：A kind of system of silica modified magnesia
Preparation Method comprising following step：
1) by magnesia calcination processing, ball milling obtains magnesium oxide powder after calcining, takes a certain amount of magnesia evenly dispersed
In organic solvent, magnesia magma is formed；
2) a certain amount of tetraethyl orthosilicate is added in organic solvent, stirs evenly to form tetraethyl orthosilicate solution；
A certain amount of ammonium hydroxide is added in organic solvent, stirs evenly to form catalyst solution；
3) tetraethyl orthosilicate solution and catalyst solution are added dropwise in magnesia magma simultaneously with certain speed,
And be stirred continuously, after being stirred to react a period of time, washing and drying treatment is to get to silica modified magnesium oxide powder.
By said program, the calcination temperature described in step 1) is 1000-1600 DEG C, soaking time 0-4h, after ball milling
The average grain diameter of magnesia is less than 3 μm, and the content of magnesia is 0.5-1.0g/ml in magnesia magma.
By said program, the calcined crystalline temperature described in step 1) is 1200-1400 DEG C, soaking time 1-2h, ball
The average grain diameter of magnesia after mill is 0.1-1 μm.
By said program, step 1) and 2) described in solvent be in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol one
Kind or a variety of mixing.
By said program, the weight ratio of tetraethyl orthosilicate and organic solvent described in step 2) is 1:2-1:6.
By said program, the weight ratio of ammonium hydroxide and solvent described in step 3) is 1:5-1:10.
By said program, the step 4) rate of addition is 1-5 seconds/drop, and the mixing time is 12-48h, and described washes
It is that deionization is washed 2-3 times to wash drying process, and absolute ethyl alcohol is washed 1-3 times, 60-120 DEG C of dry 12-24h.
Silica modified magnesia obtained by above-mentioned any one preparation method.The silica modified magnesia of gained
Applied to using magnesia as the bone renovating material of raw material.
Using above-mentioned technical proposal the beneficial effects of the present invention are：
1) the silica modified magnesia grain size that prepared by this method is small, and the residual quantity of magnesia can be reduced in application,
Ensure pH value when material degradation, helps to improve its bio-compatible performance；
2) silica modified magnesia prepared by this method can adjust the cladding of silica in application as needed
Degree can greatly meet clinical requirement；
3) the use of silica modified magnesia is bone cement prepared by raw material, the silicon ion that when degradation discharges can promote
Skeletonization；
4) other retarder need not be added when it is applied, and help to maintain its excellent biocompatibility.
Description of the drawings
Fig. 1 is the transmission electron microscope picture (TEM) of the silica modified magnesia in embodiment 1.
Specific implementation mode
Below by specific implementation, invention is further explained, and however, the present invention is not limited to these examples.
Embodiment 1
1) magnesia is heated to 1400 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 1 μm, weighs 5g magnesium oxide dispersions
In 10ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 1.5ml tetraethyl orthosilicates is taken to be added in 9ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 3s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 12 hours at 60 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 2
1) magnesia is heated to 1200 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 0.4 μm, weighs 5g magnesia point
It dissipates in 8ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 2.5ml tetraethyl orthosilicates is taken to be added in 10ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 3s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 12 hours at 60 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 3
1) magnesia is heated to 1400 DEG C and keeps the temperature 1 hour, levigate average grain diameter is 1 μm, weighs 5g magnesium oxide dispersions
In 8ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 2.0ml tetraethyl orthosilicates is taken to be added in 8ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 8ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 5s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 12 hours at 40 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 4
1) magnesia is heated to 1350 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 1 μm, weighs 5g magnesium oxide dispersions
In 7ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 3.0ml tetraethyl orthosilicates is taken to be added in 8ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 2ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 2s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react for 24 hours, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 24 hours at 40 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 5
1) magnesia is heated to 1200 DEG C and keeps the temperature 1 hour, levigate average grain diameter is 0.3 μm, weighs 5g magnesia point
It dissipates in 10ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 2ml tetraethyl orthosilicates is taken to be added in 4ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 5ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 1s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react for 24 hours, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 12 hours at 40 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 6
1) magnesia is heated to 1600 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 1 μm, weighs 5g magnesium oxide dispersions
In 10ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 1.5ml tetraethyl orthosilicates is taken to be added in 9ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 1s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 12 hours at 40 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 7
1) magnesia is heated to 1300 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 0.5 μm, weighs 5g magnesia point
It dissipates in 10ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 2ml tetraethyl orthosilicates is taken to be added in 10ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 2ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 5s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 24 hours at 60 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 8
1) magnesia is heated to 1400 DEG C and keeps the temperature 2 hours, levigate average grain diameter is 1 μm, weighs 5g magnesium oxide dispersions
In 5ml ethyl alcohol, stirring forms magnesium oxide suspension；
2) another that 2ml tetraethyl orthosilicates is taken to be added in 12ml ethyl alcohol, it stirs evenly to form tetraethyl orthosilicate solution；
3) another that 1ml ammonium hydroxide is taken to be added in 10ml ethyl alcohol, it stirs evenly to form catalyst solution；
4) tetraethyl orthosilicate solution and catalyst solution are added in magnesia magma simultaneously with the speed of 3s/ drops,
It is used in combination blender to be stirred continuously, after being stirred to react 12h, after reaction solution is centrifuged, sediment is washed with deionized twice,
It is washed twice again with absolute ethyl alcohol, is dried 24 hours at 40 DEG C, that is, silica modified magnesium oxide powder is prepared.
Embodiment 9
Embodiment 4 silica modified magnesium oxide powder 3g, potassium dihydrogen phosphate 8g, calcium dihydrogen phosphate 1g are weighed, fully
It is uniformly mixed, obtains bone renovating material solid phase, distilled water is solidify liquid, and solid liquid phase is mixed evenly, hardening time 26min.
A kind of preparation method and applications of silica modified magnesia disclosed by the invention, those skilled in the art can
By using for reference present disclosure, the appropriate links such as material and route that change are realized, material of the invention and method only introductory section weight
It tests and illustrates present disclosure with part exemplary embodiments, but these examples are not intended to limit protection scope of the present invention.
Claims (9)
1. a kind of preparation method of silica modified magnesia comprising following step：
1) by magnesia calcination processing, ball milling obtains magnesium oxide powder after calcining, and a certain amount of magnesia is taken to be dispersed in
In solvent, magnesia magma is formed；
2) a certain amount of tetraethyl orthosilicate is added in organic solvent, stirs evenly to form tetraethyl orthosilicate solution；By one
Quantitative ammonium hydroxide is added in organic solvent, stirs evenly to form catalyst solution；
3) tetraethyl orthosilicate solution and catalyst solution are added dropwise in magnesia magma simultaneously with certain speed, not
Disconnected stirring, after being stirred to react a period of time, washing and drying treatment is to get to silica modified magnesium oxide powder.
2. the preparation method of silica modified magnesia according to claim 1, which is characterized in that described in step 1)
Calcination temperature is 1000-1600 DEG C, soaking time 0-4h, and the average grain diameter of the magnesia after ball milling is less than 3 μm, and magnesia is outstanding
The content of magnesia is 0.5-1.0g/ml in supernatant liquid.
3. the preparation method of silica modified magnesia according to claim 2, which is characterized in that described in step 1)
Calcined crystalline temperature is 1200-1400 DEG C, soaking time 1-2h, and the average grain diameter of the magnesia after ball milling is 0.1-1 μm.
4. the preparation method of silica modified magnesia according to claim 1, which is characterized in that step 1) and 2) institute
The solvent stated is one or more mixing in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol.
5. the preparation method of silica modified magnesia according to claim 1, which is characterized in that described in step 2)
The weight ratio of tetraethyl orthosilicate and organic solvent is 1:2-1:6.
6. the preparation method of silica modified magnesia according to claim 1, which is characterized in that described in step 3)
The weight ratio of ammonium hydroxide and solvent is 1:5-1:10.
7. the preparation method of silica modified magnesia according to claim 1, which is characterized in that the step 4) drop
Acceleration is 1-5 seconds/drop, and the mixing time is 12-48h, and the washing and drying treatment is that deionization is washed 2-3 times, nothing
Water-ethanol is washed 1-3 times, 60-120 DEG C of dry 12-24h.
8. according to the silica modified magnesia obtained by claim 1-7 any one preparation methods.
9. the silica modified magnesia obtained by claim 8 is applied to using magnesia as the bone renovating material of raw material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233012A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Electrical-grade magnesium oxide powder and preparation method thereof |
| CN112742341A (en) * | 2019-10-30 | 2021-05-04 | 中国石油化工股份有限公司 | Magnesium oxide-silicon oxide composite with core-shell structure and preparation method thereof |
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|---|---|---|---|---|
| CN101550344A (en) * | 2008-12-20 | 2009-10-07 | 青岛科技大学 | Method for preparing magnesium hydroxide/silicon dioxide composite inorganic flame retardant |
| CN104341808A (en) * | 2014-11-05 | 2015-02-11 | 海南大学 | Room-temperature self-curing inorganic phosphate anti-corrosion paint as well as preparing method and use method of paint |
| CN104357043A (en) * | 2014-11-24 | 2015-02-18 | 北京大学工学院包头研究院 | Fluorescent material as well as preparation method and application thereof |
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2018
- 2018-03-13 CN CN201810205456.XA patent/CN108341607B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550344A (en) * | 2008-12-20 | 2009-10-07 | 青岛科技大学 | Method for preparing magnesium hydroxide/silicon dioxide composite inorganic flame retardant |
| CN104341808A (en) * | 2014-11-05 | 2015-02-11 | 海南大学 | Room-temperature self-curing inorganic phosphate anti-corrosion paint as well as preparing method and use method of paint |
| CN104357043A (en) * | 2014-11-24 | 2015-02-18 | 北京大学工学院包头研究院 | Fluorescent material as well as preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233012A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Electrical-grade magnesium oxide powder and preparation method thereof |
| CN111233012B (en) * | 2018-11-28 | 2021-10-08 | 中国科学院大连化学物理研究所 | Electrical-grade magnesium oxide powder and preparation method thereof |
| CN112742341A (en) * | 2019-10-30 | 2021-05-04 | 中国石油化工股份有限公司 | Magnesium oxide-silicon oxide composite with core-shell structure and preparation method thereof |
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