CN106115744B - 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 PDF

Info

Publication number
CN106115744B
CN106115744B CN201610458559.8A CN201610458559A CN106115744B CN 106115744 B CN106115744 B CN 106115744B CN 201610458559 A CN201610458559 A CN 201610458559A CN 106115744 B CN106115744 B CN 106115744B
Authority
CN
China
Prior art keywords
nahco
ultra
fine
particle
ethanol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201610458559.8A
Other languages
Chinese (zh)
Other versions
CN106115744A (en
Inventor
石璞
陈浪
刘跃军
伍文宗
刘小超
姜黎
孙鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan University of Technology
Original Assignee
Hunan University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan University of Technology filed Critical Hunan University of Technology
Priority to CN201610458559.8A priority Critical patent/CN106115744B/en
Publication of CN106115744A publication Critical patent/CN106115744A/en
Application granted granted Critical
Publication of CN106115744B publication Critical patent/CN106115744B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

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 the mixed solution is added in ethanol and recrystallized, obtain ultra-fine NaHCO3Particle.The ultra-fine NaHCO prepared using method provided by the invention3The size of particle is small and Size Distribution is narrower, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 94%~97% of total number of particles.By ultra-fine NaHCO provided by the invention3Particle is applied to prepare microcellular foam material, can effectively improve the mechanical property of microcellular foam material.

Description

A kind of ultra-fine NaHCO3Particle and its preparation method and application
Technical field
The present invention relates to ultra fine compound field, more 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 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 the characteristics of high.
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.The interval method of forming can obtain the foam structure of high quality, but life be present Produce the shortcomings of very long cycle, small product size and shape are limited, it is difficult to practical application.Supercritical CO2Continuous extrusion and injection The method of forming can be with continuous production, but the shortcomings of special equipment is particularly expensive, abscess is larger, cell size is relatively unmanageable be present, Limit microcellular foam material large-scale promotion and application.
Conventional foaming method is to prepare microcellular foam material using general chemistry foaming agent, and equipment is relatively easy, but is sent out It is undesirable to steep effect.Sodium acid carbonate (NaHCO3) be used as a kind of typical inorganic chemical foaming agent, have raw material be easy to get, price it is low It is honest and clean, decompose when heat absorption, product CO2In the polymer the advantages that soluble diffusion, especially it does not have toxicity, is more suitable for it Applied to fields such as foamed product packagings.But commercially available NaHCO3Particle size is bigger, generally hundreds of microns；Existing skill Typically by mechanical crushing method, freeze-drying, spray drying process to NaHCO in art3Particle carries out micronization processes, but uses NaHCO after the refinement of these methods3Particle size is still larger, and generally several microns, microcellular foam material is prepared as foaming agent When foaming effect it is still undesirable.
The content of the invention
It is an object of the invention to provide a kind of ultra-fine NaHCO3Particle and its preparation method and application.Carried using the present invention Ultra-fine NaHCO prepared by the method for confession3The size of particle is small and uniform, can effectively improve 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 the step (1) obtains is added in ethanol and recrystallized, obtain ultra-fine NaHCO3Grain Son.
Preferably, NaHCO in the step (1)3, dispersant and water mass ratio be (4~10)：(0.4~1)： 100.
Preferably, dispersant includes lauryl sodium sulfate or polyvinyl alcohol in the step (1).
Preferably, ethanol and the volume ratio of step (1) reclaimed water are (8~14) in the step (2)：1.
Preferably, mixed solution is added in ethanol in the step (2) be in stir speed (S.S.) be 800~1400r/ Carried out under conditions of min.
Preferably, mixed solution is added in ethanol in the step (2) is carried out under conditions of -8~40 DEG C.
Preferably, the pan feeding speed being added to mixed solution in ethanol in the step (2) is 1~4mL/min.
The invention provides ultra-fine NaHCO prepared by above-mentioned preparation method3Particle, granularity are the ultra-fine of 100~200nm NaHCO3Particle accounts for ultra-fine NaHCO3The 94%~97% of total number of particles.
The invention provides ultra-fine NaHCO prepared by above-mentioned preparation method3It is ultra-fine described in particle or above-mentioned technical proposal NaHCO3Application of the particle in microcellular foam material.
Preferably, using modifying agent by the ultra-fine NaHCO3Particle is used to prepare microcellular foam material after being modified；
Wherein, the modifying agent includes stearic acid, magnesium stearate, urea, 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 the mixed solution is added in ethanol and recrystallized, obtain ultra-fine NaHCO3Particle.Using this hair Ultra-fine NaHCO prepared by the method for bright offer3The size of particle is small and Size Distribution is narrower, and the embodiment of the present invention 1 shows, The ultra-fine NaHCO prepared using method provided by the invention3The particle mean size of particle is 143.2nm, and particle size is mostly distributed In the range of 100~200nm, granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 94% of total number of particles ~97%.
By ultra-fine NaHCO provided by the invention3Particle is applied to prepare microcellular foam material, can effectively improve micropore hair The mechanical property of foam material.Microcellular foam material and the power of unexpanded polypropylene material in the embodiment of the present invention to being prepared Performance is learned to be tested, the results showed that, the tensile strength of material and elongation at break have a small amount of decline after foaming, decline respectively 9.6% and 6.7%；And impact strength improves 47.8%, bending strength improves 20.2%.All things considered, using the present invention Microcellular foam material prepared by the method for offer shows preferable mechanical property.
Brief description of the drawings
Fig. 1 is NaHCO3The scanning electron microscope (SEM) photograph of commercial goods；
Fig. 2 is ultra-fine NaHCO prepared by embodiment 13The scanning electron microscope (SEM) photograph of particle；
Fig. 3 is ultra-fine NaHCO prepared by embodiment 13The particle size distribution figure of particle；
Fig. 4 is the scanning electron microscope (SEM) photograph of microcellular foam material prepared by embodiment 6；
Fig. 5 is the cell size distribution block diagram of microcellular foam material prepared by embodiment 6；
Fig. 6 is the schematic diagram of the self-control agitating device that inwall sets dividing plate in the present invention；
Fig. 7 is the pictorial diagram of the self-control agitating device that inwall sets dividing plate in the present invention.
Embodiment
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 the step (1) obtains is added in ethanol and recrystallized, obtain ultra-fine NaHCO3Grain Son.
It is provided by the invention to prepare ultra-fine NaHCO3The method of particle, it is small and uniform ultra-fine that size can be obtained NaHCO3Particle, by the ultra-fine NaHCO3Particle is applied to prepare microcellular foam material, can effectively improve 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 the raw material NaHCO3Source there is no special restriction, using NaHCO well known to those skilled in the art3Commercial goods.In the present invention In, the dispersant preferably includes lauryl sodium sulfate or polyvinyl alcohol.In the present invention, the number of the polyvinyl alcohol is divided equally Son amount is preferably 16000~20000, more preferably 17500~18500.
In the present invention, the raw material NaHCO3, dispersant and water mass ratio be preferably (4~10)：(0.4~1)： 100, more preferably (6~8)：(0.6~0.8)：100.The formation of crystal particles includes crystal nucleation and crystal is grown up two and walked 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 final size of strong influence particle, therefore, solute raw material NaHCO3Mass concentration it is larger when be advantageous to produce big mistake Saturation degree, and then produce smaller NaHCO3Particle.
The present invention is for described by raw material NaHCO3, dispersant and water the no special requirement of mixing, using this area The technical scheme of mixing known to technical staff.The present invention is preferably by raw material NaHCO3Mixed with water, obtain NaHCO3It is water-soluble Liquid, then by the NaHCO3The aqueous solution and dispersant, obtain mixed solution.In the present invention, by the raw material NaHCO3 When being mixed with water, it is preferred to use magnetic stirring apparatus heating stirring, to help raw material NaHCO3Dissolved in water.The present invention is for institute Stating the stir speed (S.S.) of magnetic stirring apparatus and heating-up temperature does not have special requirement, is used to help using well known to those skilled in the art Help raw material NaHCO3The stir speed (S.S.) and heating-up temperature dissolved in water.
The mixed solution is added in ethanol by the present invention to be recrystallized, and obtains ultra-fine NaHCO3Particle.In this hair In bright, the volume ratio of the ethanol and water is preferably (8~14)：1, more preferably (10~12)： 1.
The mixed solution is preferably added to ethanol by the present invention under conditions of stir speed (S.S.) is 800~1400r/min 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.) The mixed solution is added in ethanol under conditions of min, stops stirring until all adding.In the present invention, it is described Stir speed (S.S.) is preferably 1000~1200r/min.In the present invention, the self-control agitating device is specifically by people in the art Agitating device container inner wall sets dividing plate known to member, impulsive force when being stirred with increase, makes stirring more violent.Fig. 6 is this hair Bright middle inwall sets the schematic diagram of the self-control agitating device of dividing plate, and Fig. 7 is the self-control stirring dress that inwall sets dividing plate in the present invention The pictorial diagram put.Larger stir speed (S.S.) enhances two alternate microcosmic mixing, and then can promote two alternate mass transfers And diffusion velocity, solution can in a short time become more uniformly, and high degree of supersaturation is formed, so that caused NaHCO3Particle size is smaller, Size Distribution evenly.
The mixed solution is preferably added in ethanol by the present invention under conditions of -8~40 DEG C.The present invention is for control Equipment does not have special requirement used by temperature is -8~40 DEG C, and temperature can be controlled using well known to those skilled in the art For -8~40 DEG C of equipment.In an embodiment of the present invention, ethanol is specifically controlled using low-temperature cooling fluid circulating pump Temperature is -8~40 DEG C, and then the mixed solution is added in ethanol.In the present invention, the temperature of the control ethanol is excellent Elect -5~30 DEG C as, more preferably -2~20, most preferably 0~10 DEG C.Higher temperature can aggravate the motion of particle, increase Add the chance of interparticle collision, promote crystal to grow up；Simultaneously higher temperature can decline the surface energy of particle, be easily caused grain Son occurs to reunite and aggegation.Therefore relatively low temperature is advantageous to prepare the less NaHCO of size3Particle.
The pan feeding speed that mixed solution is added in ethanol is preferably 1~4mL/min by the present invention, and concretely 1,2,3 Or 4mL/min.
After the mixed solution is added in ethanol, the present invention preferably obtained material is filtered successively, washed, Dry and grind, obtain ultra-fine NaHCO3Particle.The present invention is for the no special requirement of filtering, using art technology The technical scheme of filtering known to personnel.Present invention preferably employs vacuum filtration to realize sediment and liquid in resulting material Separation.
After completing the filtering, the sediment filter cake that preferred pair of the present invention obtains is washed.The present invention washes for described No special requirement is washed, using the technical scheme of washing well known to those skilled in the art.Present invention preferably employs second Alcohol is by obtained sediment Washing of Filter Cake 2~3 times.
After completing the washing, the washing material that preferred pair of the present invention obtains is dried.The present invention is for the drying There is no special requirement, using the technical scheme of drying well known to those skilled in the art.The present invention will preferably obtain Washing material is dried in vacuo.In the present invention, the vacuum drying temperature is preferably 35~45 DEG C；The vacuum drying Time be preferably 10~14h.
After completing the drying, the dried material that preferred pair of the present invention obtains is ground, and obtains ultra-fine NaHCO3Grain Son.The present invention does not have special requirement for the grinding operation, using the technical side of grinding well known to those skilled in the art Case.Present invention preferably employs mechanical lapping.
Present invention also offers ultra-fine NaHCO prepared by a kind of above-mentioned preparation method3Particle, granularity are 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 above-mentioned technical proposal Ultra-fine NaHCO3Application of the particle in microcellular foam material.
Present invention preferably employs modifying agent by the ultra-fine NaHCO3Particle is used to prepare microporous foam material after being modified Material, wherein, the modifying agent preferably includes stearic acid, magnesium stearate, urea, calcium stearate or zinc sulfate.In the present invention, adopt With modifying agent by the ultra-fine NaHCO3It is to improve ultra-fine NaHCO that particle, which is modified,3The hot property of particle.The present invention is right In described to ultra-fine NaHCO3The method that particle is modified does not have special requirement, using use well known to those skilled in the art In the ultra-fine NaHCO of improvement3The 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, it is described by ultra-fine NaHCO3The method that particle is modified, preferably include following Step：
By the ultra-fine NaHCO3Particle, modifying agent and solvent mixing, after the solvent is volatilized, by obtained dry materials, Grinding, obtain the ultra-fine NaHCO of modification3Particle.
In the present invention, the 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, it is described Solvent preferably includes ether or ethanol.
The present invention is by the ultra-fine NaHCO3Particle, modifying agent and solvent mixing.The present invention is for described by ultra-fine NaHCO3 The no special requirement of operation of particle, modifying agent and solvent mixing, using the technology of mixing well known to those skilled in the art Scheme.The present invention preferably first modifying agent is mixed with solvent, then again with the ultra-fine NaHCO3Mix particles.The present invention It is preferred that under agitation by the ultra-fine NaHCO3Particle, modifying agent and solvent mixing.The present invention does not have for the stirring Special requirement, help to make that solid-liquid is well mixed, the technology of the stirring of solvent volatilization using well known to those skilled in the art Scheme.
After the solvent is volatilized, the present invention by obtained dry materials, grinding, obtain modification ultra-fine NaHCO3Particle.This Invention is for the no special requirement of the drying, using the technical scheme of drying well known to those skilled in the art.This The material that invention obtains after preferably solvent is volatilized is placed in baking oven and dried.In the present invention, the temperature of the drying is preferably 35~45 DEG C；The time of the drying is preferably 10~20min.
After completing the drying, the dried material that preferred pair of the present invention obtains is ground, and obtains the ultra-fine of modification NaHCO3Particle.The present invention does not have special requirement for the grinding operation, using grinding well known to those skilled in the art Technical scheme.Present invention preferably employs mechanical lapping.
Obtain the ultra-fine NaHCO of the modification3After particle, the present invention is preferably by modified ultra-fine NaHCO3Particle is used to make Standby microcellular foam material.The present invention does not have special requirement for preparing the method for microcellular foam material, using art technology The method for being used to prepare microcellular foam material known to personnel.Present invention preferably employs injection foaming method to prepare microporous foam Material.In the present invention, prepare the microcellular foam material and preferably include following steps：
By polymeric material, the ultra-fine NaHCO of modification3Particle and white oil mixing, dry, then entered using injection foaming method Row fretting map, obtains microcellular foam material.
The present invention is by polymeric material, the ultra-fine NaHCO of modification3Particle and white oil mixing, dry.In the present invention, institute State polymeric material, the ultra-fine NaHCO of modification3The mass ratio of particle and white oil is preferably 100：(3~6)：(0.3~0.7), More preferably 100：(4~5)：(0.4~0.6), most preferably 100： 4.5：0.5.The present invention is for the polymeric material Species does not have special requirement, using the polymeric material well known to those skilled in the art for being used to prepare expanded material. In the present invention, the polymeric material preferably includes polypropylene, polyethylene, polystyrene, polyvinyl chloride or ethyl vinyl acetate second Alkene copolymer.
The present invention is for described by polypropylene, the ultra-fine NaHCO of modification3The operation of particle and white oil mixing is no special It is required that the technical scheme using mixing well known to those skilled in the art.The present invention preferably first mixes polypropylene and white oil Close, be placed in high-speed mixer, after stirring 4~6min under 600~1000r/min, add modified ultra-fine NaHCO3Particle, Continue after stirring 4~6min under 600~1000r/min, obtain mixed material.
Obtain the ultra-fine NaHCO of polypropylene, white oil and modification3It is of the invention by the mixture after the mixed material of particle Expect drying.Invention is for the no special requirement of the drying, using the technical scheme of drying well known to those skilled in the art .Obtained material is preferably placed in baking oven and dried by the present invention.In the present invention, the temperature of the drying be preferably 35~ 45℃；The time of the drying is preferably 10~14h.
After completing the drying, present invention preferably employs injection foaming method to carry out fretting map, obtains microcellular foam material.This Operation no special requirement of the invention to the injection foaming method, using 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 the injection foaming method is：Injection pressure 40MPa, Each section of injection speed is respectively one section of 5mm/s, two sections of 20mm/s, three sections of 20mm/s, four sections of 5mm/s, and each area's gun barrel temperature is distinguished For 180 DEG C of nozzle, 190 DEG C of 4th area, 190 DEG C of 3rd area, 190 DEG C of 2nd area, 175 DEG C, dwell pressure 50MPa of an area, 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.It is aobvious So, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the reality in the present invention Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, is all belonged to In the scope of protection of the invention.
The ultra-fine NaHCO is prepared in following examples of the present invention3NaHCO needed for particle3Raw material is commercially available NaHCO3 Product.
Embodiment 1
(1) NaHCO is pressed3, lauryl sodium sulfate and water mass ratio be 10：1：100 meters, by NaHCO3Mix, adopt with water With magnetic stirring apparatus heating stirring, by NaHCO3Dissolving, obtains NaHCO3The aqueous solution, then by the NaHCO3The aqueous solution is with dividing Powder mixes, and obtains mixed solution.
(2) 1400mL ethanol is placed in the self-control agitating device that inwall sets dividing plate, using low-temperature cooling fluid circulating pump Control ethanol temperature be -5 DEG C, stir speed (S.S.) be 1100r/min under conditions of by mixed solution described in step (1) with 1mL/min pan feeding speed is added in ethanol, stops stirring until all adding.
(3) material that step (2) obtains is filtered by vacuum, ethanol wash 2 times, by obtained washing material 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 is characterized, as shown in Fig. 1 and Fig. 2. Fig. 1 is commercially available NaHCO3The scanning electron microscope (SEM) photograph of product, it can be seen that commercially available NaHCO3NaHCO in product3Block, shape is presented in particle Shape is irregular, and particle size size is extremely uneven, and size distribution ranges are 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 ultra-fine NaHCO prepared by embodiment 13Particle size substantially subtracts It is small, and Size Distribution is more uniform.
The ultra-fine NaHCO prepared using Particle Size Analyzer to embodiment 13Particle carries out particle size test, test result As shown in Figure 3.Fig. 3 is ultra-fine NaHCO prepared by embodiment 13The particle size distribution figure of particle, from the figure 3, it may be seen that embodiment 1 The ultra-fine NaHCO prepared3The average-size of particle is 143.2nm, and a particle size range only occurs, and particle size mostly divides For cloth in the range of 100~200nm, granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3Total number of particles 97%.
Embodiment 2
(1) NaHCO is pressed3, lauryl sodium sulfate and water mass ratio be 8：0.8：100 meters, by NaHCO3Mixed with water, Using magnetic stirring apparatus heating stirring, by NaHCO3Dissolving, obtains NaHCO3The aqueous solution, then by the NaHCO3The aqueous solution with Dispersant, obtain mixed solution.
(2) 800mL ethanol is placed in the self-control agitating device that inwall sets dividing plate, using 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 Min pan feeding speed is added in ethanol, stops stirring until all adding.
(3) material that step (2) obtains is filtered by vacuum, ethanol wash 3 times, by obtained washing material at 35 DEG C Lower vacuum drying 14h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO that method according to embodiment 1 is prepared to embodiment 23Particle is characterized, and acquired results are with implementing The characterization result of example 1 is consistent, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 95% of total number of particles.
Embodiment 3
(1) NaHCO is pressed3, lauryl sodium sulfate and water mass ratio be 10：0.9：100 meters, by NaHCO3Mixed with water Close, using magnetic stirring apparatus heating stirring, by NaHCO3Dissolving, obtains NaHCO3The aqueous solution, then by the NaHCO3The aqueous solution With dispersant, mixed solution is obtained.
(2) 800mL ethanol is placed in the self-control agitating device that inwall sets dividing plate, using 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 be added in ethanol, until all add i.e. stop stirring.
(3) material that step (2) obtains is filtered by vacuum, ethanol wash 3 times, by obtained washing material at 35 DEG C Lower vacuum drying 13h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO that method according to embodiment 1 is prepared to embodiment 33Particle is characterized, and acquired results are with implementing The characterization result of example 1 is consistent, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 97% of total number of particles.
Embodiment 4
(1) NaHCO is pressed3, polyethylene alcohol and water mass ratio be 8：1.1：100 meters, by NaHCO3Mixed with water, using magnetic Power agitator heating stirring, by NaHCO3Dissolving, obtains NaHCO3The aqueous solution, then by the NaHCO3The aqueous solution and dispersant Mixing, obtains mixed solution.
(2) 1400mL ethanol is placed in the self-control agitating device that inwall sets dividing plate, using low-temperature cooling fluid circulating pump It is 40 DEG C to control ethanol temperature, by mixed solution described in step (1) with 1mL/ under conditions of stir speed (S.S.) is 800r/min Min pan feeding speed is added in ethanol, stops stirring until all adding.
(3) material that step (2) obtains is filtered by vacuum, ethanol wash 3 times, by obtained washing material at 40 DEG C Lower vacuum drying 11h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO that method according to embodiment 1 is prepared to embodiment 43Particle is characterized, and acquired results are with implementing The characterization result of example 1 is consistent, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 95% of total number of particles.
Embodiment 5
(1) NaHCO is pressed3, polyethylene alcohol and water mass ratio be 4：0.5：100 meters, by NaHCO3Mixed with water, using magnetic Power agitator heating stirring, by NaHCO3Dissolving, obtains NaHCO3The aqueous solution, then by the NaHCO3The aqueous solution and dispersant Mixing, obtains mixed solution.
(2) 1200mL ethanol is placed in the self-control agitating device that inwall sets dividing plate, using low-temperature cooling fluid circulating pump Control ethanol temperature be 20 DEG C, stir speed (S.S.) be 1000r/min under conditions of by mixed solution described in step (1) with 4mL/min pan feeding speed is added in ethanol, stops stirring until all adding.
(3) material that step (2) obtains is filtered by vacuum, ethanol wash 3 times, by obtained washing material at 40 DEG C Lower vacuum drying 10h, obtains ultra-fine NaHCO after grinding3Particle.
The ultra-fine NaHCO that method according to embodiment 1 is prepared to embodiment 53Particle is characterized, and acquired results are with implementing The characterization result of example 1 is consistent, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3The 94% of total number of particles.
Embodiment 6
(1) the ultra-fine NaHCO prepared by embodiment 13The mass ratio of particle, stearic acid and ether is 100： 60：12 meters, Stearic acid and ether are mixed, then again with the ultra-fine NaHCO3Mix particles, stir to solvent after volatilizing, the thing that will be obtained Material is placed in baking oven, 40 DEG C of dry 15min, and the ultra-fine NaHCO of modification is obtained after grinding3Particle；
(2) by polypropylene, the ultra-fine NaHCO of modification3The 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 under 800r/min, add the ultra-fine of step (1) described modification NaHCO3Particle, continue after stirring 5min under 800r/min, obtain mixed material.
(3) mixed material that step (2) obtains is placed in baking oven, 40 DEG C of dry 12h, then entered using injection foaming method Row fretting map, obtains microcellular foam material；The concrete operations parameter of the injection foaming method is：Injection pressure 40MPa, each section of note Firing rate degree is respectively one section of 5mm/s, two sections of 20mm/s, three sections of 20mm/s, four sections of 5mm/s, and each area's gun barrel temperature is respectively nozzle 180 DEG C, 190 DEG C of 4th area, 190 DEG C of 3rd area, 190 DEG C of 2nd area, 175 DEG C, dwell pressure 50MPa, cool time 20s of an area.
Microcellular foam material prepared by embodiment 6 is characterized, as shown in Figure 4.Fig. 4 is micropore prepared by embodiment 6 The scanning electron microscope (SEM) photograph of expanded material, it can be seen that foam structure is good in microcellular foam material, is hole-closing structure, substantially in ball Shape；And it is preliminary as can be seen that the size of abscess is very small, uniformity coefficient is also high.
Using the scanning electron microscope (SEM) photograph of microcellular foam material, pass through the particle size statistical softwares pair of Nano Measurer 1.2 Microcellular foam material abscess-size is counted.Drawn through statistical software analysis, as little as 0.47 μm of abscess average-size, abscess Dimensional standard variance is only 0.162 μm, illustrates the abscess-size degree of scatter of microcellular foam material prepared by embodiment 6 very Concentrate small, abscess-size pole.Fig. 5 is the cell size distribution block diagram of microcellular foam material prepared by embodiment 6, can be more straight See ground and find out that the size of the microcellular foam material is small, Size Distribution is concentrated.
The microcellular foam material and the mechanical property of unexpanded polypropylene material prepared to embodiment 6 is tested, as a result 1 is shown in Table, method of testing is as follows：
1) tensile property：Tensile property measure is carried out according to GB/T1040-92, draw speed 50mm/min, is tested Carried out on microcomputer controlled electronic universal tester.
2) bending property：Bending property measure is carried out according to GB/T9341-2000, is tested in the omnipotent examination of microcomputer controlled electronic Test on machine and carry out, pressing speed 2.0mm/min, positioning moves 6mm.
3) impact property：According to ISO179-2:1997 carry out cantilever beam impact strength measure, test in plastics Charpy impact Carried out on testing machine.
Microcellular foam material and the mechanical experimental results of unexpanded polypropylene material prepared by the embodiment 6 of table 1
As it can be seen from table 1 the tensile strength of material and elongation at break have a small amount of decline after foaming, decline respectively 9.6% and 6.7%；And impact strength improves 47.8%, bending strength improves 20.2%.It is prepared by all things considered, embodiment 6 Microcellular foam material show preferable mechanical property.
The ultra-fine NaHCO prepared it can be seen from above example and result of the test using method provided by the invention3 The size of particle is small and Size Distribution is narrower, and granularity is 100~200nm ultra-fine NaHCO3Particle accounts for ultra-fine NaHCO3Grain The 94%~97% of sub- sum.By ultra-fine NaHCO provided by the invention3Particle is applied to prepare microcellular foam material, Neng Gouyou Effect improves the mechanical property of microcellular foam material.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (6)

  1. A kind of 1. 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 the step (1) obtains is added in ethanol and recrystallized, obtain ultra-fine NaHCO3Particle；
    NaHCO in the step (1)3, dispersant and water mass ratio be (4~8)：(0.4~1)：100；
    Ethanol and the volume ratio of step (1) reclaimed water are (8~14) in the step (2)：1；
    Mixed solution, which is added in ethanol, in the step (2) is entered under conditions of stir speed (S.S.) is 800~1400r/min OK；
    Mixed solution, which is added in ethanol, in the step (2) is carried out under conditions of -8~40 DEG C.
  2. 2. preparation method according to claim 1, it is characterised in that dispersant includes dodecyl in the step (1) Sodium sulphate or polyvinyl alcohol.
  3. 3. preparation method according to claim 1, it is characterised in that mixed solution is added to second in the step (2) Pan feeding speed in alcohol is 1~4mL/min.
  4. A kind of 4. ultra-fine NaHCO that in claims 1 to 3 prepared by preparation method described in any one3Particle, it is characterised in that grain Spend the ultra-fine NaHCO for 100~200nm3Particle accounts for ultra-fine NaHCO3The 94%~97% of total number of particles.
  5. 5. the ultra-fine NaHCO described in claim 43Application of the particle in microcellular foam material.
  6. 6. application according to claim 5, it is characterised in that using modifying agent by the ultra-fine NaHCO3Particle is changed Property after be used for prepare microcellular foam material；
    Wherein, the modifying agent includes stearic acid, magnesium stearate, urea, calcium stearate or zinc sulfate.
CN201610458559.8A 2016-06-22 2016-06-22 A kind of ultra-fine NaHCO3Particle and its preparation method and application Expired - Fee Related CN106115744B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610458559.8A CN106115744B (en) 2016-06-22 2016-06-22 A kind of ultra-fine NaHCO3Particle and its preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610458559.8A CN106115744B (en) 2016-06-22 2016-06-22 A kind of ultra-fine NaHCO3Particle and its preparation method and application

Publications (2)

Publication Number Publication Date
CN106115744A CN106115744A (en) 2016-11-16
CN106115744B true CN106115744B (en) 2017-12-01

Family

ID=57267964

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610458559.8A Expired - Fee Related CN106115744B (en) 2016-06-22 2016-06-22 A kind of ultra-fine NaHCO3Particle and its preparation method and application

Country Status (1)

Country Link
CN (1) CN106115744B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102618786B1 (en) 2016-07-20 2023-12-29 솔베이(소시에떼아노님) 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
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

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1010305B (en) * 1984-07-17 1990-11-07 索维尔公司 Process for preparing organic base from aqueous solution of alkali metal bicarbonate and hydrochloride organic base containing nitrogenous
FR2576589B1 (en) * 1985-01-30 1987-03-27 Solvay PROCESS FOR THE MANUFACTURE OF DENSE ANHYDROUS SODIUM CARBONATE AND DENSE ANHYDROUS SODIUM CARBONATE OBTAINED BY THIS PROCESS
FR2590561B1 (en) * 1985-11-25 1988-01-29 Solvay PROCESS FOR THE PREPARATION OF AN AQUEOUS SOLUTION OF SODIUM CHLORIDE AND PROCESS FOR THE PRODUCTION OF SODIUM BICARBONATE
CN1027750C (en) * 1991-10-05 1995-03-01 化工部制碱工业研究所 Process and apparatus for preparing 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
CN104326493B (en) * 2014-10-14 2015-11-18 江苏金象赛瑞化工科技有限公司 A kind of take sodium bicarbonate as the technique of raw material production Soda Ash Danse
CN105540618B (en) * 2015-12-23 2017-03-29 湖南工业大学 A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material

Also Published As

Publication number Publication date
CN106115744A (en) 2016-11-16

Similar Documents

Publication Publication Date Title
CN106115744B (en) A kind of ultra-fine NaHCO3Particle and its preparation method and application
CN103387691B (en) A kind of hollow polystyrene plastic pellet and its preparation method and application
CN105080439A (en) Microspheres with high fluorescence intensity and preparation method for microspheres
CN103103629B (en) Fullerene-polymer composite nanofiber and preparation method thereof
CN106237993B (en) A kind of Fe3O4The preparation method of@MOF-199@C18 nanocomposite
CN209953036U (en) Sulphuric acid granule agitating unit with screening function
CN107377993B (en) A kind of metal nanometer line, dispersion liquid and preparation method thereof
CN104072656B (en) A kind of method preparing ferroso-ferric oxide-composite magnetic microsp Heres
CN105107462A (en) Preparation method for oxidized graphene-metal organic framework nano composite material
CN103980506B (en) A kind of preparation method of the magnetic microsphere based on PLEG
CN106916315A (en) Metal porous organic framework material, its preparation method and its application
CN104194003A (en) Method for preparing black monodisperse polymer microspheres
CN107930591A (en) A kind of gravity Method metal-organic solution deposition doping amino acid composite material and preparation method thereof
CN101406820B (en) Method for preparing nucleocapsid type microgel composite microsphere using polymerisable surfactant
CN105540618B (en) A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material
CN106881025B (en) Natural propolis is that the atmosphere free radical of matrix traps the preparation method of film
CN106866863A (en) A kind of preparation method of porous polymer microballoon anion filler
CN105949390A (en) Pickering malachite green molecular imprinting polymers as well as preparation method and application thereof
JP6569684B2 (en) Iron soap, method for producing the same, and thermoplastic resin composition containing the iron soap
CN110342505A (en) A kind of preparation method of parents' unsymmetric structure graphene oxide, parents' unsymmetric structure graphene oxide and its application
CN105949368A (en) Multi-responsiveness amphiphilic polymer microparticle and preparation method thereof
CN103387740B (en) A kind of hollow plastic pellet and its preparation method and application
CN109180844A (en) A kind of shaggy polystyrene microsphere and its preparation method and application
CN109485531A (en) Superfine spherical CL-20 Composite Energetic Materials and preparation method thereof
CN106179243A (en) A kind of preparation method of new dye adsorbent

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20171201

Termination date: 20190622

CF01 Termination of patent right due to non-payment of annual fee