CN106115744A - A kind of ultra-fine NaHCO3particle and its preparation method and application - Google Patents
A kind of ultra-fine NaHCO3particle and its preparation method and application Download PDFInfo
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- CN106115744A CN106115744A CN201610458559.8A CN201610458559A CN106115744A CN 106115744 A CN106115744 A CN 106115744A CN 201610458559 A CN201610458559 A CN 201610458559A CN 106115744 A CN106115744 A CN 106115744A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/24—Crystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention provides a kind of ultra-fine NaHCO3The preparation method of particle, by raw material NaHCO3, dispersant and water mixing, obtain mixed solution；Then described mixed solution is joined and ethanol carries out recrystallization, obtain ultra-fine NaHCO3Particle.Ultra-fine NaHCO prepared by the method using the present invention to provide3The size of particle is little and distribution of sizes is narrower, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 94%～97% of total number of particles.The ultra-fine NaHCO that the present invention is provided3Particle is applied to prepare microcellular foam material, it is possible to be effectively improved the mechanical property of microcellular foam material.
Description
Technical field
The present invention relates to ultra fine compound field, particularly to a kind of ultra-fine NaHCO3Particle and preparation method thereof and should
With.
Background technology
Microcellular foam material refer to abscess-size be 0.1～10 μm, cell density be 109～1012Individual/cm3Foaming material
Material.Compared with common expanded material, microcellular foam material has that density is low, heat-proof quality is excellent, soundproof effect is good and than strong
Spend high feature.
Currently, the preparation method of microcellular foam material mainly has the interval method of forming, supercritical CO2Continuous extrusion method,
Supercritical CO2Injection moulding and conventional foaming method.Intermittently the method for forming can obtain high-quality foam structure, but exists raw
The product cycle is the longest, small product size and the shortcoming such as shape is limited, it is difficult to actual application.Supercritical CO2Continuous extrusion and injection
The method of forming can produce continuously, but there is the shortcomings such as special equipment is particularly expensive, abscess is relatively big, cell size is relatively difficult to control to,
Limit microcellular foam material large-scale promotion and application.
Conventional foaming method is to use general chemistry foaming agent to prepare microcellular foam material, and equipment is relatively easy, but sends out
Bubble effect is undesirable.Sodium bicarbonate (NaHCO3) as a kind of typical inorganic chemical foaming agent, have raw material be easy to get, price low
Honest and clean, decompose time heat absorption, product CO2The advantages such as the most soluble diffusion, especially it does not has toxicity, is more suitable for it
It is applied to the fields such as foamed product packaging.But commercially available NaHCO3Particle size is bigger, the most hundreds of micron；Existing skill
In art, general mechanical crushing method, freeze-drying, the spray drying method of passing through is to NaHCO3Particle carries out micronization processes, but uses
NaHCO after the refinement of these methods3Particle size is the biggest, the most several microns, prepares microcellular foam material as foaming agent
Time foaming effect the most undesirable.
Summary of the invention
It is an object of the invention to provide a kind of ultra-fine NaHCO3Particle and its preparation method and application.Employing is the present invention carry
Ultra-fine NaHCO prepared by the method for confession3The size of particle is little and uniform, it is possible to be effectively improved the mechanics of microcellular foam material
Performance.
The invention provides a kind of ultra-fine NaHCO3The preparation method of particle, comprises the following steps:
(1) by raw material NaHCO3, dispersant and water mixing, obtain mixed solution；
(2) mixed solution that described step (1) obtains is joined ethanol carries out recrystallization, obtain ultra-fine NaHCO3Grain
Son.
Preferably, NaHCO in described step (1)3, the mass ratio of dispersant and water be (4～10): (0.4～1): 100.
Preferably, in described step (1), dispersant includes sodium lauryl sulphate or polyvinyl alcohol.
Preferably, in described step (2), ethanol is (8～14) with the volume ratio of water in step (1): 1.
Preferably, being joined in ethanol by mixed solution in described step (2) is to be 800～1400r/ in stir speed (S.S.)
Carry out under conditions of min.
Preferably, being joined in ethanol by mixed solution in described step (2) is to carry out under conditions of-8～40 DEG C.
Preferably, mixed solution joining the pan feeding speed in ethanol in described step (2) is 1～4mL/min.
The invention provides ultra-fine NaHCO prepared by above-mentioned preparation method3Particle, granularity be 100～200nm ultra-fine
NaHCO3Particle accounts for ultra-fine NaHCO3The 94%～97% of total number of particles.
The invention provides ultra-fine NaHCO prepared by above-mentioned preparation method3Ultra-fine described in particle or technique scheme
NaHCO3Particle application in microcellular foam material.
Preferably, use modifying agent by described ultra-fine NaHCO3Particle be modified after for preparing microcellular foam material；
Wherein, described modifying agent includes stearic acid, magnesium stearate, carbamide, calcium stearate or zinc sulfate.
The invention provides a kind of ultra-fine NaHCO3The preparation method of particle, by NaHCO3, dispersant and water mixing, obtain
Mixed solution；Then described mixed solution is joined and ethanol carries out recrystallization, obtain ultra-fine NaHCO3Particle.Use this
Ultra-fine NaHCO prepared by the method for bright offer3The size of particle is little and distribution of sizes is narrower, and the embodiment of the present invention 1 shows,
Ultra-fine NaHCO prepared by the method using the present invention to provide3The particle mean size of particle is 143.2nm, and particle size is mostly distributed
In the range of 100～200nm, granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 94% of total number of particles
～97%.
The ultra-fine NaHCO that the present invention is provided3Particle is applied to prepare microcellular foam material, it is possible to is effectively improved micropore and sends out
The mechanical property of foam material.To the microcellular foam material prepared and the power of unexpanded polypropylene material in the embodiment of the present invention
Performance is tested, and result shows, after foaming, hot strength and the elongation at break of material have a small amount of decline, decline respectively
9.6% and 6.7%；And impact strength improves 47.8%, bending strength improves 20.2%.All things considered, uses the present invention
Microcellular foam material prepared by the method provided shows preferable mechanical property.
Accompanying drawing explanation
Fig. 1 is NaHCO3The scanning electron microscope (SEM) photograph of commercial goods；
Fig. 2 is the ultra-fine NaHCO of embodiment 1 preparation3The scanning electron microscope (SEM) photograph of particle；
Fig. 3 is the ultra-fine NaHCO of embodiment 1 preparation3The particle size distribution figure of particle；
Fig. 4 is the scanning electron microscope (SEM) photograph of the microcellular foam material of embodiment 6 preparation；
Fig. 5 is the cell size distribution block diagram of the microcellular foam material of embodiment 6 preparation；
Fig. 6 is the schematic diagram of the self-control agitating device that inwall arranges dividing plate in the present invention；
Fig. 7 is the pictorial diagram of the self-control agitating device that inwall arranges dividing plate in the present invention.
Detailed description of the invention
The invention provides a kind of ultra-fine NaHCO3The preparation method of particle, comprises the following steps:
(1) by raw material NaHCO3, dispersant and water mixing, obtain mixed solution；
(2) mixed solution that described step (1) obtains is joined ethanol carries out recrystallization, obtain ultra-fine NaHCO3Grain
Son.
What the present invention provided prepares ultra-fine NaHCO3The method of particle, it is possible to obtain size little and the most ultra-fine
NaHCO3Particle, by described ultra-fine NaHCO3Particle is applied to prepare microcellular foam material, it is possible to be effectively improved microcellular foam material
Mechanical property.
The present invention is by raw material NaHCO3, dispersant and water mixing, obtain mixed solution.The present invention is for described raw material
NaHCO3Source there is no special restriction, use NaHCO well known to those skilled in the art3Commercial goods.In the present invention
In, described dispersant preferably includes sodium lauryl sulphate or polyvinyl alcohol.In the present invention, the number of described polyvinyl alcohol is divided equally
Son amount is preferably 16000～20000, more preferably 17500～18500.
In the present invention, described raw material NaHCO3, the mass ratio of dispersant and water be preferably (4～10): (0.4～1):
100, more preferably (6～8): (0.6～0.8): 100.The formation of crystal particles includes that crystal nucleation and crystal are grown up two and walks
Suddenly, compared with crystal growth process, the nucleation rate of crystal is more to rely on degree of supersaturation, and the nucleation rate meeting of crystal
The size that strong influence particle is final, therefore, solute raw material NaHCO3Mass concentration bigger time be conducive to producing big mistake
Saturation, and then produce smaller NaHCO3Particle.
The present invention for described by raw material NaHCO3, the mixing of dispersant and water there is no special requirement, use this area
The technical scheme of the mixing known to technical staff.The present invention is preferably by raw material NaHCO3Mix with water, obtain NaHCO3Water-soluble
Liquid, then by described NaHCO3Aqueous solution and dispersant, obtain mixed solution.In the present invention, by described raw material NaHCO3
When mixing with water, it is preferred to use magnetic stirring apparatus heated and stirred, to help raw material NaHCO3Water dissolves.The present invention is for institute
Stir speed (S.S.) and the heating-up temperature of stating magnetic stirring apparatus do not have special requirement, use well known to those skilled in the art for helping
Help raw material NaHCO3The stir speed (S.S.) dissolved in water and heating-up temperature.
Described mixed solution is joined and carries out recrystallization in ethanol by the present invention, obtains ultra-fine NaHCO3Particle.At this
In bright, described ethanol is preferably (8～14) with the volume ratio of water: 1, more preferably (10～12): 1.
Described mixed solution is preferably joined ethanol under conditions of stir speed (S.S.) is 800～1400r/min by the present invention
In.In an embodiment of the present invention, specifically ethanol is placed in self-control agitating device, is 800～1400r/ in stir speed (S.S.)
Under conditions of min, described mixed solution is joined in ethanol, until all addition i.e. stops stirring.In the present invention, described
Stir speed (S.S.) is preferably 1000～1200r/min.In the present invention, described self-control agitating device is specifically by people in the art
Agitating device container inner wall known to Yuan arranges dividing plate, to increase impulsive force during stirring, makes stirring more violent.Fig. 6 is this
Bright middle inwall arranges the schematic diagram of the self-control agitating device of dividing plate, and Fig. 7 is the self-control stirring dress that in the present invention, inwall arranges dividing plate
The pictorial diagram put.Bigger stir speed (S.S.) enhances two alternate microcosmic mixing, and then can promote two alternate quality transmission
And diffusion velocity, solution can be made at short notice to become more uniform, and form high degree of supersaturation, so that produce
NaHCO3Particle size is less, distribution of sizes evenly.
Described mixed solution is preferably joined in ethanol under conditions of-8～40 DEG C by the present invention.The present invention is for controlling
Temperature does not has special requirement by-8～40 DEG C of equipment used, and uses and well known to those skilled in the art can control temperature
For the equipment of-8～40 DEG C.In an embodiment of the present invention, low-temperature cooling fluid circulating pump is specifically used to control ethanol
Temperature is-8～40 DEG C, is then joined in ethanol by described mixed solution.In the present invention, the temperature of described control ethanol is excellent
Elect-5～30 DEG C as, more preferably-2～20, most preferably 0～10 DEG C.Higher temperature can make the motion of particle aggravate, and increases
The chance of interparticle collision, promotes that crystal is grown up；The highest temperature can make the surface of particle to decline, and is easily caused particle
Occur to reunite and coagulation.The most relatively low temperature is conducive to the NaHCO that preparation size is less3Particle.
Mixed solution is joined the pan feeding speed in ethanol and is preferably 1～4mL/min by the present invention, and concretely 1,2,3
Or 4mL/min.
After being joined in ethanol by described mixed solution, the material obtained preferably carries out filtering, washs by the present invention successively,
It is dried and grinds, obtain ultra-fine NaHCO3Particle.The present invention does not has special requirement for described filtration, uses art technology
The technical scheme of the filtration known to personnel.Present invention preferably employs vacuum filtration and realize precipitate and liquid in gained material
Separation.
After completing described filtration, the precipitate filter cake obtained preferably is washed by the present invention.The present invention washes for described
Wash and there is no special requirement, use the technical scheme of washing well known to those skilled in the art.Present invention preferably employs second
Alcohol is by the precipitate Cake Wash 2 obtained～3 times.
After completing described washing, the washing material obtained preferably is dried by the present invention.The present invention is dried for described
There is no special requirement, use dry technical scheme well known to those skilled in the art.The present invention preferably will obtain
Washing material is vacuum dried.In the present invention, described vacuum drying temperature is preferably 35～45 DEG C；Described vacuum drying
Time be preferably 10～14h.
Complete that described the dried material obtained preferably is ground by the present invention after drying, obtain ultra-fine NaHCO3Particle.
The present invention does not has special requirement for described grinding operation, uses the technical scheme of grinding well known to those skilled in the art i.e.
Can.Present invention preferably employs mechanical lapping.
Present invention also offers ultra-fine NaHCO prepared by a kind of above-mentioned preparation method3Particle, granularity is 100～200nm
Ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 94%～97% of total number of particles.
The invention provides ultra-fine NaHCO prepared by a kind of above-mentioned preparation method3Described in particle or technique scheme
Ultra-fine NaHCO3Particle application in microcellular foam material.
Present invention preferably employs modifying agent by described ultra-fine NaHCO3Particle be modified after for preparing microporous foam material
Material, wherein, described modifying agent preferably includes stearic acid, magnesium stearate, carbamide, calcium stearate or zinc sulfate.In the present invention, adopt
With modifying agent by described ultra-fine NaHCO3Particle is modified being to improve ultra-fine NaHCO3The hot property of particle.The present invention couple
In described to ultra-fine NaHCO3The method that particle is modified does not has special requirement, uses use well known to those skilled in the art
In improving ultra-fine NaHCO3The method of modifying of particle hot property.Present invention preferably employs solution cladding process to described ultra-fine
NaHCO3Particle is modified.In the present invention, described by ultra-fine NaHCO3The method that particle is modified, preferably includes following
Step:
By described ultra-fine NaHCO3Particle, modifying agent and solvent mixing, until solvent volatilize after, by the dry materials obtained,
Grind, obtain the ultra-fine NaHCO of modification3Particle.
In the present invention, described ultra-fine NaHCO3The mass ratio of particle, modifying agent and solvent is preferably 100:(55～65):
(15～25), more preferably 100:(58～62): (18～22), most preferably 100:60:20.In the present invention, described solvent
Preferably include ether or ethanol.
The present invention is by described ultra-fine NaHCO3Particle, modifying agent and solvent mixing.The present invention for described by ultra-fine NaHCO3
The operation of particle, modifying agent and solvent mixing does not has special requirement, uses the technology of mixing well known to those skilled in the art
Scheme.Modifying agent is the most first mixed by the present invention with solvent, the most again with described ultra-fine NaHCO3Mix particles.The present invention
The most under agitation by described ultra-fine NaHCO3Particle, modifying agent and solvent mixing.The present invention does not has for described stirring
Special requirement, uses the technology of the stirring contributing to and making solid-liquid mix homogeneously, solvent volatilize well known to those skilled in the art
Scheme.
After solvent volatilizees, the present invention, by the dry materials obtained, grinding, obtains the ultra-fine NaHCO of modification3Particle.This
Invent and special requirement is not had for described being dried, use dry technical scheme well known to those skilled in the art.This
The material that invention obtains after preferably being volatilized by solvent is placed in baking oven and is dried.In the present invention, described dry temperature is preferably
35～45 DEG C；The described dry time is preferably 10～20min.
Complete that described the dried material obtained preferably is ground by the present invention after drying, obtain the ultra-fine of modification
NaHCO3Particle.The present invention does not has special requirement for described grinding operation, uses grinding well known to those skilled in the art
Technical scheme.Present invention preferably employs mechanical lapping.
Obtain the ultra-fine NaHCO of described modification3After particle, the present invention is preferably by modified ultra-fine NaHCO3Particle is used for making
Standby microcellular foam material.The present invention does not has special requirement for the method preparing microcellular foam material, uses art technology
The method being used for preparing microcellular foam material known to personnel.Present invention preferably employs injection foaming method and prepare microporous foam
Material.In the present invention, prepare described microcellular foam material and preferably include following steps:
By polymeric material, modified ultra-fine NaHCO3Particle and white oil mix, are dried, and then use injection foaming method to enter
Row fretting map, obtains microcellular foam material.
The present invention is by polymeric material, modified ultra-fine NaHCO3Particle and white oil mix, are dried.In the present invention, institute
State polymeric material, modified ultra-fine NaHCO3The mass ratio of particle and white oil is preferably 100:(3～6): (0.3～0.7), more
It is preferably 100:(4～5): (0.4～0.6), most preferably 100:4.5:0.5.The present invention is for the kind of described polymeric material
Class does not has special requirement, uses the polymeric material for preparing expanded material well known to those skilled in the art.?
In the present invention, described polymeric material preferably includes polypropylene, polyethylene, polystyrene, polrvinyl chloride or ethene-vinyl acetate
Copolymer.
The present invention for described by polypropylene, modified ultra-fine NaHCO3It is special that the operation of particle and white oil mixing does not has
Requirement, uses the technical scheme of mixing well known to those skilled in the art.Polypropylene and white oil are the most first mixed by the present invention
Close, be placed in high-speed mixer, after stirring 4～6min under 600～1000r/min, add the ultra-fine NaHCO of modification3Particle,
After continuing to stir 4～6min under 600～1000r/min, obtain mixed material.
Obtain the ultra-fine NaHCO of polypropylene, white oil and modification3After the mixed material of particle, the present invention is by described mixture
Material is dried.Invent and special requirement is not had for described being dried, use dry technical scheme well known to those skilled in the art
?.The material obtained preferably is placed in baking oven and is dried by the present invention.In the present invention, described dry temperature be preferably 35～
45℃；The described dry time is preferably 10～14h.
Complete described after drying, present invention preferably employs injection foaming method and carry out fretting map, obtain microcellular foam material.This
Invent the operation to described injection foaming method and there is no special requirement, use injection foaming method well known to those skilled in the art
Technical scheme.In an embodiment of the present invention, the concrete operations parameter of described injection foaming method is: injection pressure 40MPa,
Each section of injection speed is respectively one section of 5mm/s, two-stage nitration 20mm/s, three sections of 20mm/s, four sections of 5mm/s, and each district gun barrel temperature is respectively
For 180 DEG C of nozzle, 190 DEG C of 4th district, 190 DEG C of 3rd district, 190 DEG C of 2nd district, 175 DEG C of a district, dwell pressure 50MPa, cool time
20s。
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.Aobvious
So, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the reality in the present invention
Execute example, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all belong to
In the scope of protection of the invention.
Following example of the present invention are prepared described ultra-fine NaHCO3NaHCO needed for particle3Raw material is commercially available NaHCO3
Product.
Embodiment 1
(1) NaHCO is pressed3, the mass ratio of sodium lauryl sulphate and water be 10:1:100 meter, by NaHCO3Mix with water, adopt
Use magnetic stirring apparatus heated and stirred, by NaHCO3Dissolve, obtain NaHCO3Aqueous solution, then by described NaHCO3Aqueous solution with point
Powder mixes, and obtains mixed solution.
(2) 1400mL ethanol is placed in the self-control agitating device that inwall arranges dividing plate, uses low-temperature cooling fluid circulating pump
Control ethanol temperature and be-5 DEG C, by mixed solution described in step (1) with 1mL/ under conditions of stir speed (S.S.) is 1100r/min
The pan feeding speed of min joins in ethanol, until all addition i.e. stops stirring.
(3) material that step (2) obtains is carried out vacuum filtration, washing with alcohol 2 times, by the washing material that obtains at 40 DEG C
Lower vacuum drying 12h, obtains ultra-fine NaHCO after grinding3Particle.
Ultra-fine NaHCO prepared by embodiment 13Particle and commercially available NaHCO3Product characterizes, as depicted in figs. 1 and 2.
Fig. 1 is commercially available NaHCO3The scanning electron microscope (SEM) photograph of product, it can be seen that commercially available NaHCO3NaHCO in product3Particle presents bulk, shape
Shape is irregular, and particle size size is the most uneven, and size distribution ranges is wide, from 5～50 μm.Fig. 2 is that embodiment 1 is made
Standby ultra-fine NaHCO3The scanning electron microscope (SEM) photograph of particle, it can be seen that the ultra-fine NaHCO of embodiment 1 preparation3Particle size substantially subtracts
Little, and distribution of sizes is more uniform.
Use the ultra-fine NaHCO that embodiment 1 is prepared by Particle Size Analyzer3Particle carries out particle size test, test result
As shown in Figure 3.Fig. 3 is the ultra-fine NaHCO of embodiment 1 preparation3The particle size distribution figure of particle, from the figure 3, it may be seen that embodiment 1
The ultra-fine NaHCO of preparation3The average-size of particle is 143.2nm, and only occurs in that a particle size range, and particle size mostly divides
Cloth is in the range of 100～200nm, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3Total number of particles
97%.
Embodiment 2
(1) NaHCO is pressed3, the mass ratio of sodium lauryl sulphate and water be 8:0.8:100 meter, by NaHCO3Mix with water,
Use magnetic stirring apparatus heated and stirred, by NaHCO3Dissolve, obtain NaHCO3Aqueous solution, then by described NaHCO3Aqueous solution with
Dispersant, obtains mixed solution.
(2) 800mL ethanol is placed in the self-control agitating device that inwall arranges dividing plate, uses low-temperature cooling fluid circulating pump control
Ethanol temperature processed is-8 DEG C, by mixed solution described in step (1) with 2mL/ under conditions of stir speed (S.S.) is 1400r/min
The pan feeding speed of min joins in ethanol, until all addition i.e. stops stirring.
(3) material that step (2) obtains is carried out vacuum filtration, washing with alcohol 3 times, by the washing material that obtains at 35 DEG C
Lower vacuum drying 14h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO according to the method for embodiment 1 prepared by embodiment 23Particle characterizes, acquired results and enforcement
Example 1 characterization result is consistent, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 95% of total number of particles.
Embodiment 3
(1) NaHCO is pressed3, the mass ratio of sodium lauryl sulphate and water be 10:0.9:100 meter, by NaHCO3Mix with water,
Use magnetic stirring apparatus heated and stirred, by NaHCO3Dissolve, obtain NaHCO3Aqueous solution, then by described NaHCO3Aqueous solution with
Dispersant, obtains mixed solution.
(2) 800mL ethanol is placed in the self-control agitating device that inwall arranges dividing plate, uses low-temperature cooling fluid circulating pump control
Ethanol temperature processed is 15 DEG C, by mixed solution described in step (1) with 1mL/min under conditions of stir speed (S.S.) is 800r/min
Pan feeding speed join in ethanol, until all addition i.e. stops stirring.
(3) material that step (2) obtains is carried out vacuum filtration, washing with alcohol 3 times, by the washing material that obtains at 35 DEG C
Lower vacuum drying 13h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO according to the method for embodiment 1 prepared by embodiment 33Particle characterizes, acquired results and enforcement
Example 1 characterization result is consistent, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 97% of total number of particles.
Embodiment 4
(1) NaHCO is pressed3, the mass ratio of polyethylene alcohol and water be 8:1.1:100 meter, by NaHCO3Mix with water, use magnetic
Power agitator heated and stirred, by NaHCO3Dissolve, obtain NaHCO3Aqueous solution, then by described NaHCO3Aqueous solution and dispersant
Mixing, obtains mixed solution.
(2) 1400mL ethanol is placed in the self-control agitating device that inwall arranges dividing plate, uses low-temperature cooling fluid circulating pump
Controlling ethanol temperature is 40 DEG C, by mixed solution described in step (1) with 1mL/ under conditions of stir speed (S.S.) is 800r/min
The pan feeding speed of min joins in ethanol, until all addition i.e. stops stirring.
(3) material that step (2) obtains is carried out vacuum filtration, washing with alcohol 3 times, by the washing material that obtains at 40 DEG C
Lower vacuum drying 11h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO according to the method for embodiment 1 prepared by embodiment 43Particle characterizes, acquired results and enforcement
Example 1 characterization result is consistent, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 95% of total number of particles.
Embodiment 5
(1) NaHCO is pressed3, the mass ratio of polyethylene alcohol and water be 4:0.5:100 meter, by NaHCO3Mix with water, use magnetic
Power agitator heated and stirred, by NaHCO3Dissolve, obtain NaHCO3Aqueous solution, then by described NaHCO3Aqueous solution and dispersant
Mixing, obtains mixed solution.
(2) 1200mL ethanol is placed in the self-control agitating device that inwall arranges dividing plate, uses low-temperature cooling fluid circulating pump
Controlling ethanol temperature is 20 DEG C, by mixed solution described in step (1) with 4mL/ under conditions of stir speed (S.S.) is 1000r/min
The pan feeding speed of min joins in ethanol, until all addition i.e. stops stirring.
(3) material that step (2) obtains is carried out vacuum filtration, washing with alcohol 3 times, by the washing material that obtains at 40 DEG C
Lower vacuum drying 10h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO according to the method for embodiment 1 prepared by embodiment 53Particle characterizes, acquired results and enforcement
Example 1 characterization result is consistent, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 94% of total number of particles.
Embodiment 6
(1) by the ultra-fine NaHCO of embodiment 1 preparation3The mass ratio of particle, stearic acid and ether is 100:60:12 meter, will
Stearic acid and ether mixing, the most again with described ultra-fine NaHCO3Mix particles, stirs after volatilizing to solvent, the material that will obtain
It is placed in baking oven, 40 DEG C of dry 15min, after grinding, obtains the ultra-fine NaHCO of modification3Particle；
(2) polypropylene, modified ultra-fine NaHCO are pressed3The mass ratio of particle and white oil is 100:4.5:0.5 meter, by poly-third
Alkene and white oil mixing are placed in high-speed mixer, after stirring 5min, add the ultra-fine of step (1) described modification under 800r/min
NaHCO3Particle, after continuing to stir 5min under 800r/min, obtains mixed material.
(3) mixed material that step (2) obtains is placed in baking oven, 40 DEG C of dry 12h, then uses injection foaming method to enter
Row fretting map, obtains microcellular foam material；The concrete operations parameter of described injection foaming method is: injection pressure 40MPa, each section of note
Firing rate degree is respectively one section of 5mm/s, two-stage nitration 20mm/s, three sections of 20mm/s, four sections of 5mm/s, and each district gun barrel temperature is respectively nozzle
180 DEG C, 190 DEG C of 4th district, 190 DEG C of 3rd district, 190 DEG C of 2nd district, 175 DEG C of a district, dwell pressure 50MPa, cool time 20s.
Microcellular foam material prepared by embodiment 6 is characterized, as shown in Figure 4.Fig. 4 is the micropore of embodiment 6 preparation
The scanning electron microscope (SEM) photograph of expanded material, it can be seen that in microcellular foam material, foam structure is good, for hole-closing structure, substantially in ball
Shape；And preliminary it can be seen that the size of abscess is the least, uniformity coefficient is the highest.
Use the scanning electron microscope (SEM) photograph of microcellular foam material, by Nano Measurer 1.2 particle size statistical software pair
Microcellular foam material abscess-size is added up.Through statistical software, analysis draws, abscess average-size as little as 0.47 μm, abscess chi
Very little standard variance is only 0.162 μm, illustrates that the abscess-size degree of scatter of microcellular foam material prepared by embodiment 6 is very
Little, abscess-size pole is concentrated.Fig. 5 is the cell size distribution block diagram of the microcellular foam material of embodiment 6 preparation, can be more straight
Seeing ground and find out that the size of described microcellular foam material is little, distribution of sizes is concentrated.
The microcellular foam material of embodiment 6 preparation and the mechanical property of unexpanded polypropylene material are tested, result
Being shown in Table 1, method of testing is as follows:
1) tensile property: carry out tensile property mensuration according to GB/T1040-92, draw speed is 50mm/min, tests
Carry out on microcomputer controlled electronic universal tester.
2) bending property: being curved performance measurement according to GB/T9341-2000, test is in the omnipotent examination of microcomputer controlled electronic
Testing and carry out on machine, pressing speed is 2.0mm/min, and 6mm is moved in location.
3) impact property: carrying out cantilever beam impact strength mensuration according to ISO179-2:1997, test is at plastics Charpy impact
Carry out on testing machine.
The microcellular foam material of table 1 embodiment 6 preparation and the mechanical experimental results of unexpanded polypropylene material
As it can be seen from table 1 hot strength and the elongation at break of material have a small amount of decline after Fa Pao, decline respectively
9.6% and 6.7%；And impact strength improves 47.8%, bending strength improves 20.2%.All things considered, prepared by embodiment 6
Microcellular foam material show preferable mechanical property.
By above example and result of the test it can be seen that use ultra-fine NaHCO prepared by the method for present invention offer3Grain
The size of son is little and distribution of sizes is narrower, and granularity is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3Particle
The 94%～97% of sum.The ultra-fine NaHCO that the present invention is provided3Particle is applied to prepare microcellular foam material, it is possible to effectively
Improve the mechanical property of microcellular foam material.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a ultra-fine NaHCO3The preparation method of particle, comprises the following steps:
(1) by raw material NaHCO3, dispersant and water mixing, obtain mixed solution；
(2) mixed solution that described step (1) obtains is joined ethanol carries out recrystallization, obtain ultra-fine NaHCO3Particle.
Preparation method the most according to claim 1, it is characterised in that NaHCO in described step (1)3, dispersant and water
Mass ratio is (4～10): (0.4～1): 100.
Preparation method the most according to claim 1, it is characterised in that in described step (1), dispersant includes dodecyl
Sodium sulfate or polyvinyl alcohol.
Preparation method the most according to claim 1, it is characterised in that ethanol and water in step (1) in described step (2)
Volume ratio is (8～14): 1.
Preparation method the most according to claim 1, it is characterised in that mixed solution is joined second in (2) by described step
Alcohol is carry out under conditions of stir speed (S.S.) is 800～1400r/min.
Preparation method the most according to claim 1 or 5, it is characterised in that mixed solution is joined in (2) by described step
Ethanol is carry out under conditions of-8～40 DEG C.
Preparation method the most according to claim 1, it is characterised in that mixed solution is joined second in (2) by described step
Pan feeding speed in alcohol is 1～4mL/min.
8. the ultra-fine NaHCO that in a claim 1～7 prepared by preparation method described in any one3Particle, it is characterised in that grain
Degree is the ultra-fine NaHCO of 100～200nm3Particle accounts for ultra-fine NaHCO3The 94%～97% of total number of particles.
9. the ultra-fine NaHCO described in claim 83Particle application in microcellular foam material.
Application the most according to claim 9, it is characterised in that use modifying agent by described ultra-fine NaHCO3Particle changes
It is used for after property preparing microcellular foam material；
Wherein, described modifying agent includes stearic acid, magnesium stearate, carbamide, calcium stearate or zinc sulfate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264746A (en) * | 2018-10-12 | 2019-01-25 | 河南精康制药有限公司 | A kind of preparation method of pharmaceutical grade sodium bicarbonate |
| CN112500833A (en) * | 2020-12-11 | 2021-03-16 | 河南理工大学 | Inert gas driven cold aerosol explosion suppressant and preparation method thereof |
| US11421094B2 (en) | 2016-07-20 | 2022-08-23 | Solvay Sa | Functionalized particulate bicarbonate as blowing agent, foamable polymer composition containing it, and its use in manufacturing a thermoplastic foamed polymer |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86100688A (en) * | 1985-01-30 | 1986-07-30 | 索尔维公司 | The manufacture method of heavy anhydrous sodium carbonate and the heavy anhydrous sodium carbonate that makes with this method |
| CN85105969A (en) * | 1984-07-17 | 1987-02-25 | 索维尔公司 | Produce the method for organic bases and sodium bicarbonate by the hydrochloride of bicarbonate aqueous solution and nitrogenous organic base |
| CN86108737A (en) * | 1985-11-25 | 1987-08-12 | 索尔维公司 | The preparation method of sodium chloride aqueous solution and the production method of sodium bicarbonate |
| CN1059883A (en) * | 1991-10-05 | 1992-04-01 | 化工部制碱工业研究所 | Produce the method and apparatus of sodium bicarbonate |
| CN1780671A (en) * | 2003-04-29 | 2006-05-31 | 阿克佐诺贝尔股份有限公司 | Processes involving the use of antisolvent crystallisation |
| CN102815752A (en) * | 2012-09-24 | 2012-12-12 | 湖南工业大学 | Novel quaternary layered double hydroxide (LDHs), its preparation method and application thereof |
| CN103012857A (en) * | 2012-12-06 | 2013-04-03 | 湖南工业大学 | Microcrystalline cellulose and polycaprolactone reinforced starch-based full-biodegradable blending material and preparation method thereof |
| CN104326493A (en) * | 2014-10-14 | 2015-02-04 | 江苏金象赛瑞化工科技有限公司 | Process using sodium bicarbonate as raw material to produce heavy soda ash |
| CN105540618A (en) * | 2015-12-23 | 2016-05-04 | 湖南工业大学 | Sodium bicarbonate, preparation method thereof and application of sodium bicarbonate in foam materials |
-
2016
- 2016-06-22 CN CN201610458559.8A patent/CN106115744B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105969A (en) * | 1984-07-17 | 1987-02-25 | 索维尔公司 | Produce the method for organic bases and sodium bicarbonate by the hydrochloride of bicarbonate aqueous solution and nitrogenous organic base |
| CN86100688A (en) * | 1985-01-30 | 1986-07-30 | 索尔维公司 | The manufacture method of heavy anhydrous sodium carbonate and the heavy anhydrous sodium carbonate that makes with this method |
| CN86108737A (en) * | 1985-11-25 | 1987-08-12 | 索尔维公司 | The preparation method of sodium chloride aqueous solution and the production method of sodium bicarbonate |
| CN1059883A (en) * | 1991-10-05 | 1992-04-01 | 化工部制碱工业研究所 | Produce the method and apparatus of sodium bicarbonate |
| CN1780671A (en) * | 2003-04-29 | 2006-05-31 | 阿克佐诺贝尔股份有限公司 | Processes involving the use of antisolvent crystallisation |
| CN102815752A (en) * | 2012-09-24 | 2012-12-12 | 湖南工业大学 | Novel quaternary layered double hydroxide (LDHs), its preparation method and application thereof |
| CN103012857A (en) * | 2012-12-06 | 2013-04-03 | 湖南工业大学 | Microcrystalline cellulose and polycaprolactone reinforced starch-based full-biodegradable blending material and preparation method thereof |
| CN104326493A (en) * | 2014-10-14 | 2015-02-04 | 江苏金象赛瑞化工科技有限公司 | Process using sodium bicarbonate as raw material to produce heavy soda ash |
| CN105540618A (en) * | 2015-12-23 | 2016-05-04 | 湖南工业大学 | Sodium bicarbonate, preparation method thereof and application of sodium bicarbonate in foam materials |
Non-Patent Citations (2)
| Title |
|---|
| 叶明泉等: ""超细粒子及其复合技术在冷气溶胶灭火剂中的应用"", 《南京理工大学学报》 * |
| 李菲等: ""反溶剂重结晶法制备超细碳酸氢钾粉体"", 《现代化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11421094B2 (en) | 2016-07-20 | 2022-08-23 | Solvay Sa | Functionalized particulate bicarbonate as blowing agent, foamable polymer composition containing it, and its use in manufacturing a thermoplastic foamed polymer |
| CN109264746A (en) * | 2018-10-12 | 2019-01-25 | 河南精康制药有限公司 | A kind of preparation method of pharmaceutical grade sodium bicarbonate |
| CN112500833A (en) * | 2020-12-11 | 2021-03-16 | 河南理工大学 | Inert gas driven cold aerosol explosion suppressant and preparation method thereof |
| CN112500833B (en) * | 2020-12-11 | 2023-06-02 | 河南理工大学 | Inert gas-driven cold aerosol explosion suppressant and preparation method thereof |
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