CN105540618B - A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material - Google Patents
A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material Download PDFInfo
- Publication number
- CN105540618B CN105540618B CN201510979661.8A CN201510979661A CN105540618B CN 105540618 B CN105540618 B CN 105540618B CN 201510979661 A CN201510979661 A CN 201510979661A CN 105540618 B CN105540618 B CN 105540618B
- Authority
- CN
- China
- Prior art keywords
- nahco
- sodium bicarbonate
- preparation
- present
- air bubble
- 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
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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- 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
- C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
-
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention provides a kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material.The present invention is prepared for nano-calcium carbonate hydrogen sodium using air bubble liquid-membrane interface method, and concrete preparation method is as follows：By water, NaHCO3, Nano-meter SiO_22, thickening agent and cement blowing agent mix, obtain in air bubble liquid-membrane, and liquid film wall, also having a large amount of less bubbles by stirring；NaHCO when being dried3The crystallization on air bubble liquid-membrane interface is separated out, and the bubble in the middle of liquid film hinders NaHCO3Grow up, so as to obtain the NaHCO of small particle3.The NaHCO that the present invention is provided3For 80nm width, the laminated structure of 280nm length, hence it is evident that less than commercially available NaHCO3Size (5 μm～100 μm), decomposition temperature is than commercially available NaHCO3It is much lower, can be used for the excellent microcellular foam material of processability.The preparation method simple process that the present invention is provided, less energy consumption, it is adaptable to industrialized production.
Description
Technical field
The present invention relates to technical field of inorganic, more particularly to a kind of sodium bicarbonate and preparation method thereof and sodium bicarbonate
Application in expanded material.
Background technology
Sodium bicarbonate (NaHCO3) sodium bicarbonate is commonly called as, it is a kind of more important inorganic chemical product, is widely used in
The fields such as light industry, medicine, weaving and fine chemistry industry.Due to the competition in market, some applications are to NaHCO3The requirement of quality is more next
It is higher, such as high molecular foam material field.NaHCO3As a kind of inorganic type foaming agent, with heat absorption, product during nontoxic, decomposition
Thing CO2In the polymer the advantages of soluble diffusion.Therefore, in foaming agent field, especially should be noted safe field (such as
Need and food or human contact), NaHCO3Play an important role.
At present, sodium carbonate (Na is generally adopted both at home and abroad2CO3) and CO2NaHCO is produced in reaction3, be divided into gas-solid phase method and
Gas and liquid phase method.NaHCO3In crystallization, as crystal quickly can grow, therefore bulky grain product is easily produced, to the greatest extent
Pipe carries out Mechanical Method refinement to product, and most particle diameters still can only achieve 60～100 mesh.Using the NaHCO of big particle diameter3As
Foaming agent, can only obtain wide-aperture expanded material.It is well known that abscess is bigger, the performance of the aspect such as expanded material mechanics is equal
It is poorer.And microcellular foam material, due to the size of micropore it is less than the flaw size inside polymeric material, though therefore foam after
So density have dropped, but mechanical properties decrease is seldom, or even some indexs (such as impact strength) can be greatly improved, and can be significantly
Degree reduces the heat conductivity of polymer, improves the heat preserving heat insulating noise insulation effect of expanded material, and these characteristics have high application
Value.
Microcellular foam material to be prepared, needs the foaming agent that particle diameter is little.But obtain the little NaHCO of particle diameter3Not a duck soup.Closely
Nian Lai, specially to NaHCO3Research report in terms of granularity refinement is less.Li Maoqiang is prepared for using solution spray evaporation technique
NaHCO3Powder, the powder particles made are little, spherical in shape, powder diameter Distribution between 0.8～20 μm, wherein less than 10 μm
Granule account for 92%.Zhang Yuqian employs directly freezed, vacuum evaporation freezing and three kinds of freeze-dryings of spray chilling and is prepared for
Ultra-fine NaHCO3, wherein with spray chilling effect preferably, powder particles are 2.26 μm.Although can be prepared using said method
The little NaHCO of particle diameter3Particle, but its particle diameter is still micron level.Therefore, how a kind of smaller NaHCO is provided3Particle
Become this area technical problem urgently to be resolved hurrily.
The content of the invention
It is an object of the invention to provide a kind of sodium bicarbonate and preparation method thereof and sodium bicarbonate are in expanded material
Application.The present invention prepares small particle sodium bicarbonate by air bubble liquid-membrane method, and method is easy, low cost.What the present invention was provided
Sodium bicarbonate size is Nano grade, and compared with commercially available sodium bicarbonate, smaller, decomposition temperature is lower.
The invention provides a kind of preparation method of sodium bicarbonate, comprises the following steps：
(1) by NaHCO3With water, Nano-meter SiO_22Mixed solution is mixed to get with thickening agent；
(2) mixed solution that the step (1) is obtained is mixed with foaming agent, obtains air bubble liquid-membrane；
(3) air bubble liquid-membrane for obtaining step (2) is dried, and obtains sodium bicarbonate.
Preferably, in the step (1) water volume and NaHCO3And Nano-meter SiO_22Mass ratio be：100mL:(8～12)
g:(8～14) g.
Preferably, in the step (1), thickening agent and the volume ratio of water are 1:(10～50).
Preferably, in the step (2), foaming agent and the volume ratio of water are (3～6):50.
Preferably, the Nano-meter SiO_22Particle diameter be 10～100nm.
Preferably, the thickening agent is water-based thickener.
Preferably, the foaming agent is surfactant-based foaming agent.
Preferably, the baking temperature in the step (3) is 45～55 DEG C, and drying time is 10～14h.
Present invention also offers the sodium bicarbonate prepared according to a kind of above-mentioned preparation method, the sodium bicarbonate size is to receive
Meter level is other.
Preferably, sodium bicarbonate structure in the form of sheets, size is：Long 200～400nm, wide 60～100nm.
Preferably, also contain Nano-meter SiO_2 in the sodium bicarbonate2。
Present invention also offers sodium bicarbonate described in a kind of above-mentioned technical proposal or preparing according to above-mentioned preparation method
Application in expanded material.
The invention provides a kind of air bubble liquid-membrane interface method prepares NaHCO3Method.The present invention is by NaHCO3Solution
Middle addition foaming agent, produces substantial amounts of air bubble liquid-membrane, NaHCO after stirring3On liquid film interface crystallize, due to liquid film it is very thin, and
And also with the presence of many less bubbles in liquid film, they can hinder NaHCO3The growth of crystal, has reached reduction NaHCO3Granularity
Purpose, method is simple, easy to operate.
Present invention also offers NaHCO prepared by a kind of above-mentioned preparation method3.The NaHCO that the present invention is provided3Size is to receive
Meter level is other, in the form of sheets structure, and size is：Long 200～400nm, wide 60～100nm, decomposition temperature are significantly less than commercially available NaHCO3。
Present invention also offers described in a kind of above-mentioned technical proposal or above-mentioned preparation method prepare NaHCO3In foaming material
Application in material.The NaHCO that the present invention is provided3Size is Nano grade, can be used for the excellent microcellular foam material of processability.
Description of the drawings
Fig. 1 is commercially available NaHCO3Polarized light microscopy pattern before grinding；
Fig. 2 is commercially available NaHCO3Polarized light microscopy pattern after grinding；
Fig. 3 is commercially available NaHCO3SEM photograph；
Fig. 4 is commercially available NaHCO3DSC curve figure；
The polarized light microscopy pattern of dried air bubble liquid-membranes of the Fig. 5 to prepare in embodiment 1；
The polarized light microscopy pattern of dried air bubble liquid-membranes of the Fig. 6 to prepare in embodiment 3；
Fig. 7 is the microphotograph that Fig. 6 amplifies 4 times；
The polarized light microscopy pattern of air bubble liquid-membranes of the Fig. 8 to prepare in embodiment 7；
The polarized light microscopy pattern of air bubble liquid-membranes of the Fig. 9 to prepare in embodiment 10；
Figure 10 is the NaHCO for preparing in embodiment 113TEM photos；
Figure 11 is the NaHCO for preparing in embodiment 113DSC curve figure；
The polarized light microscopy pattern of air bubble liquid-membranes of the Figure 12 to prepare in embodiment 11；
Figure 13 is the NaHCO for preparing in embodiment 113The expanded material impact fracture surface SEM photograph of preparation；
The polarized light microscopy pattern of air bubble liquid-membranes of the Figure 14 to prepare in embodiment 12.
Specific embodiment
The invention provides a kind of preparation method of sodium bicarbonate, comprises the following steps：
(1) by NaHCO3With water, Nano-meter SiO_22Mixed solution is mixed to get with thickening agent；
(2) mixed solution that the step (1) is obtained is mixed with foaming agent, obtains air bubble liquid-membrane；
(3) air bubble liquid-membrane for obtaining step (2) is dried, and obtains sodium bicarbonate.
The present invention is by NaHCO3With water, Nano-meter SiO_22Mixed solution is mixed to get with thickening agent.The present invention is mixed to described preparation
The operation for closing solution does not have special restriction, using the technical scheme for preparing mixed solution well known to those skilled in the art i.e.
Can.The present invention is preferably by NaHCO3It is soluble in water, obtain NaHCO3Aqueous solution, then by the NaHCO3Aqueous solution successively with receive
Rice SiO2Mix with thickening agent, obtain mixed solution.In the present invention, the volume and NaHCO of the water3And Nano-meter SiO_22Matter
Amount ratio preferably 100mL:(8～12) g:(8～14) g, more preferably 100mL:(9～11) g:(10～13) g；The thickening agent
1 is preferably with the volume ratio of water:(10～50), more preferably 1:(13～25), most preferably 1：(15～19).
In the present invention, the Nano-meter SiO_22Particle diameter be preferably 10～100nm, more preferably 10～30nm.At this
In bright, the Nano-meter SiO_22With thixotropic transformation, increase can the viscosity of system in low sheraing effect or under standing, it is possible to increase
Liquid feeding film-strength, the Film strength for especially heating up when being dried, so that air bubble liquid-membrane stable existence in the dry state, and
Retain substantial amounts of minute bubbles in making air pocket, these minute bubbles hinder growing up for sodium bicarbonate crystal.
In the present invention, the thickening agent is preferably water-based thickener.In an embodiment of the present invention, the thickening agent can
Specially polyurethaness thickening agent or water miscible polyacrylate.In the present invention, the thickening agent is liquid, and its effect is
Solution viscosity is adjusted, obtains that cell diameter is little, high-quality soap bubble of uniform size at normal temperatures.
The mixed solution for obtaining is mixed by the present invention with foaming agent, obtains air bubble liquid-membrane.The present invention prepares bubble to described
The operation of liquid film does not have special restriction, using the technical scheme of foaming well known to those skilled in the art.The present invention is excellent
The mixed solution and foaming agent are prepared air bubble liquid-membrane under conditions of stirring by choosing, and the stir speed (S.S.) is preferably 300
～500r/min, mixing time are preferably 20～25min.In the present invention, the foaming agent is preferably (3 with the volume ratio of water
～6):50, more preferably (3.5～5)：50.In the present invention, the foaming agent is preferably surfactant-based foaming agent.
In embodiments of the invention, the foaming agent can be specially animal class cement blowing agent.In the present invention, the work of the foaming agent
With being to form tough and tensile, whippy air bubble liquid-membrane.In the present invention, the body of the foaming agent and water described in above-mentioned technical proposal
Product is than being preferably (3～6):50, more preferably (3.5～5)：50.
The air bubble liquid-membrane for obtaining is dried by the present invention, obtains sodium bicarbonate.The present invention is not special to the drying process
Restriction, using the technical scheme of drying well known to those skilled in the art.In the present invention, the drying is preferably dried
It is dry, in an embodiment of the present invention, the air bubble liquid-membrane can be placed in baking oven and be dried.In the present invention, the baking temperature
Preferably 45～55 DEG C, more preferably 48～52 DEG C, the drying time is preferably 10～14h, more preferably 11～13h.
After completing the drying, product after drying is preferably ground by the present invention, obtains sodium bicarbonate.The present invention is to institute
Stating grinding operation does not have special restriction, using the technical scheme of grinding well known to those skilled in the art.The present invention is excellent
Choosing adopts mechanical lapping.
Present invention also offers sodium bicarbonate prepared by a kind of above-mentioned preparation method, the size of the sodium bicarbonate is nanometer
Rank.In the present invention, the sodium bicarbonate preferably structure in the form of sheets, is preferably dimensioned to be long 200～400nm, wide by 60～
100nm, more preferably grows 250～350nm, wide 70～90nm.In the sodium bicarbonate, Nano-meter SiO_2 is preferably comprised2。
Present invention also offers the sodium bicarbonate prepared described in a kind of above-mentioned technical proposal or according to above-mentioned preparation method exists
Application in expanded material.In the present invention, the sodium bicarbonate size is Nano grade, is preferred for preparing with polymeric material
Expect the microcellular foam material for base.
In the present invention, the quality of the sodium bicarbonate is preferably 5～7% with polymeric material quality.
In the present invention, application of the sodium bicarbonate in expanded material preferably includes following steps：
(1) sodium bicarbonate for providing the present invention and stearic acid mixing post-heating, obtain mixed material；
(2) mixed material described in step (1) is mixed with polymeric material, obtains expanded material.
The present invention is by sodium bicarbonate and stearic acid mixing post-heating.The present invention is not special to the mixing and heating operation
Restriction, using it is well known to those skilled in the art mixing and heat technical scheme.In the present invention, the stearic acid
Quality be preferably polymeric material quality 2～4%；The stearic effect is to increase inorganic foaming agent and organic polymer
The compatibility between thing.In the present invention, the mixing is carried out preferably in high-speed mixer.In the present invention, the heating
Temperature is preferably 65～75 DEG C.
Mixed material is mixed by the present invention with polymeric material, obtains expanded material.The present invention does not have to the married operation
There is special restriction, using the technical scheme of mixing well known to those skilled in the art.In the present invention, the mixing is excellent
Mix in being selected in high-speed mixer, the mixing temperature is preferably 65～75 DEG C, incorporation time is preferably 10～20min.
After completing the mixing, the product for obtaining preferably is molded by the present invention, obtains expanded material.The present invention is to institute
Stating injection operation does not have special restriction, using the technical scheme of injection well known to those skilled in the art.In the present invention
In, the design parameter of the injection is preferably：80～90MPa of injection pressure, 70～80mm/s of injection speed, each section of temperature difference
For 190～200 DEG C of nozzle, 195～205 DEG C of 4th area, 195～205 DEG C of 3rd area, 185～195 DEG C of 2nd area, 165～175 DEG C of an area,
55～65MPa of pressurize, cools down 20～25s.
In order to further illustrate the present invention, the sodium bicarbonate that the present invention is provided is retouched in detail with reference to embodiment
State, but they can not be interpreted as limiting the scope of the present invention.
Due to working as NaHCO3On the liquid film of bubble during crystal growth, the space interval that air bubble is formed just can be prevented
NaHCO3Crystal is grown up and is merged, such NaHCO3Growth will be suppressed.Bubble is less, number of bubbles is more, bubble is strong
Degree bigger, bubble intensity when being heated is higher, then isolation suppresses NaHCO3The ability grown up is stronger, in theory, made
For the NaHCO for going out3Size can be less.In an embodiment of the present invention, the air bubble liquid-membrane to obtaining is tested, by bubble liquid
The quality judging NaHCO of film3Size.
Comparative example 1：
Using polarizing microscope to grinding before and after commercially available NaHCO3It is observed：Take a small amount of commercially available NaHCO3Sample tiles
On microscope slide, microscope slide is placed in into thermal station, with room temperature under observe and take pictures.Commercially available NaHCO before grinding3Pattern as shown in figure 1,
Commercially available NaHCO after grinding3Pattern is as shown in Figure 2.It can be seen that：Before grinding, commercially available NaHCO3Crystalline size is very big, crystalline size
About 50～150 μm；After grinding, commercially available NaHCO3Particle size reduction, but also considerable particle size is still left at 50 μm
It is right.
Using the common commercially available NaHCO of the desk-top SEM observations of Phenom G2 pro3Pattern.Commercially available NaHCO3SEM photograph such as
Shown in Fig. 3.As can be seen that commercially available NaHCO3Size is larger, and size pole heterogeneity, and size is 5～100 μm, and big grain
Son is in the majority, and less particle is covered on the surface of big particle.
Using differential scanning calorimeter (DSC) to commercially available NaHCO3Decomposition temperature is tested.Commercially available NaHCO3Granule
DSC curve figure is as shown in Figure 4, it can be seen that commercially available NaHCO3It is internal to contain a small amount of water of crystallization, it is heated to lose when 90.1 DEG C
Water forms a little endothermic peak；Second peak is NaHCO3Decomposition endothermic peak, non-constant width, about 110～180 DEG C, this explanation
Commercially available NaHCO3Particle size distribution range is wide；Decompose at 163.2 DEG C most fast.
Embodiment 1:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 8g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 4mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in Figure 5.
Embodiment 2:
Weigh the commercially available NaHCO of 8g3, it is dissolved in 100mL distilled water, is subsequently adding 10g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 4mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 3:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 4mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in Figure 6 and Figure 7.
Embodiment 4:
Weigh the commercially available NaHCO of 12g3, it is dissolved in 100mL distilled water, is subsequently adding 14g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 4mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 5:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 2mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 48 DEG C of oven drying 13h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 6:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 4mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 52 DEG C of oven drying 11h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 7:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 6mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, microscope slide is put
Under thermal station, with room temperature observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and in 50 DEG C of constant temperature
Observation bubbles burst and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in Figure 8.
Embodiment 8:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 8mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 45 DEG C of oven drying 14h is placed in, grinding is obtained
Sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, will
Microscope slide is placed in thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and
50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 9:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 10mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 12mL animal classes cement foamed
Bubble, with the speed stirring 25min of 420r/min, is then laid in pallet, is placed in 55 DEG C of oven drying 14h, ground by agent
Obtain sodium bicarbonate.Dried air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample and be laid in microscope slide
On, microscope slide is placed in into thermal station, with room temperature under observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min,
And in 50 DEG C of constant temperature observation bubbles bursts and crystallization situation, use software Taking Pictures recording.
Embodiment 10:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 6mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 6mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, microscope slide is put
Under thermal station, with room temperature observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and in 50 DEG C of constant temperature
Observation bubbles burst and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in Figure 9.
Embodiment 11:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 6mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 8mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.
Air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, microscope slide is put
Under thermal station, with room temperature observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and in 50 DEG C of constant temperature
Observation bubbles burst and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in figure 12.
The NaHCO prepared using transmission electron microscope observing3Pattern：A small amount of sample dispersion is taken in dehydrated alcohol, ultrasonic disperse
30 minutes, drip on sample stage, it is to be dried after be placed on TEM observe sample form.NaHCO3TEM photos such as Figure 10 institutes
Show, wherein being NaHCO at I3Particle, is Nano-meter SiO_2 at II2Particle.As can be seen that NaHCO3Particle structure in the form of sheets, size are long
For 200～400nm, a width of 60～100nm, this nanometer of NaHCO3By Nano-meter SiO_22It is coated with.
Using NaHCO of the differential scanning calorimeter (DSC) to preparation3Decomposition temperature is tested.The NaHCO of preparation3's
DSC curve figure is as shown in figure 11, it can be seen that its DSC curve has two obvious decomposition endothermic peaks at regular intervals, discloses
NaHCO3Particle size may have two kinds of different range scales.The NaHCO prepared in the present embodiment3The temperature of decomposition is all
It is significantly smaller than commercially available NaHCO3Decomposition temperature.As, after the particle diameter of material is changed into nano material, decomposition temperature can step-down.This
The NaHCO prepared in further demonstrate that the present embodiment3Particle diameter has been greatly reduced, and is mutually coincide with TEM test results.
Embodiment 12:
Weigh the commercially available NaHCO of 10g3, it is dissolved in 100mL distilled water, is subsequently adding 12g Nano-meter SiO_2s2, stirred with agitator always
Mix to uniform, add 6mL aqueous polyurethane thixotropic thickening agents, after solution is uniform, add 10mL animal class cement blowing agents,
With the speed stirring 25min of 420r/min, bubble is laid in into pallet then, 50 DEG C of oven drying 12h is placed in, grinding is obtained
Sodium bicarbonate.Air bubble liquid-membrane is observed using polarizing microscope：Take a small amount of sample to be laid on microscope slide, microscope slide is put
Under thermal station, with room temperature observe and take pictures；Setting program heats up, and rises to 50 DEG C with the speed of 10 DEG C/min, and in 50 DEG C of constant temperature
Observation bubbles burst and crystallization situation, use software Taking Pictures recording.Air bubble liquid-membrane pattern is as shown in figure 14.
The NaHCO that will be prepared in embodiment 113With stearic acid with mass ratio as 4：3 ratio is in high-speed mixer
Mixing, is warming up to 70 DEG C, after mix homogeneously, and the polypropylene for taking 70g mixture with 1kg adds high-speed mixer, in 70 DEG C of conditions
Lower mixing 15min, is drawn a design with injection machine after discharging and obtains expanded material batten, and injection design parameter is：Injection pressure 85MPa,
Injection speed 75mm/s, each section of temperature：195 DEG C of nozzle, 200 DEG C of 4th area, 200 DEG C of 3rd area, 190 DEG C of 2nd area, 170 DEG C of an area, protect
Pressure 60MPa, cools down 22s.
By above-mentioned expanded material batten and not foamed polypropylene be placed in standard environment (23 DEG C ± 2 DEG C, relative humidity
45%～55%) under adjust 48h after carry out Mechanics Performance Testing.Impact property in the present invention surveys testing equipment using Shenzhen ten thousand
The 501B-4 plastics balance weight impact testing machines of company limited are tested, and using Chalpy impact (11J), result of the test is shown in Table 1；
Tensile property is tested using 6104 microcomputer controlled electronic universal testers of CMT that China Shenzhen is newly thought carefully, rate of extension is
50mm/min, result of the test are shown in Table 2；Phenom G2 of the section after expanded material impact using Holland Phenom-world
Pro desk type scanning electronic microscopes are observed, and impact fracture surface SEM photograph is shown in Figure 13.
1 impact property of table
2 tensile property of table
| Unexpanded polypropylene | Expanded polypropylene material | |
| Tensile strength/MPa | 24.948 | 24.207 |
As can be seen from the above embodiments, the invention provides a kind of preparation small particle sodium bicarbonate of novel low-cost
Method, the preparation method provided using the present invention can obtain a large amount of high intensity uniformly, and the little bubble of cell diameter is being dried
In the case of, also many more small bubbles are present.The sodium bicarbonate size that the present invention is provided is Nano grade, with commercially available carbonic acid
Hydrogen sodium is compared, and size reduces in the order of magnitude, and decomposition temperature is lower, can be used to prepare microcellular foam material.The carbon that the present invention is provided
Cell diameter in expanded material prepared by sour hydrogen sodium is 0.4 μm～3.6 μm, compared with not foamed polymeric material, punching
Hit toughness and improve 16%, and tensile strength is basically unchanged.
The above is only the preferred embodiment of the present invention, not makees any pro forma restriction to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (11)
1. a kind of preparation method of sodium bicarbonate, comprises the following steps：
(1) by NaHCO3With water, Nano-meter SiO_22Mixed solution is mixed to get with thickening agent；
(2) mixed solution that the step (1) is obtained is mixed with foaming agent, obtains air bubble liquid-membrane；
(3) air bubble liquid-membrane for obtaining step (2) is dried, and obtains sodium bicarbonate, contains Nano-meter SiO_2 in the sodium bicarbonate2。
2. preparation method according to claim 1, it is characterised in that the volume and NaHCO of water in the step (1)3With receive
Rice SiO2Mass ratio be：100mL:(8～12) g:(8～14) g.
3. preparation method according to claim 1, it is characterised in that the volume ratio of thickening agent and water in the step (1)
For 1:(10～50).
4. preparation method according to claim 1, it is characterised in that the volume ratio of foaming agent and water in the step (2)
For (3～6):50.
5. preparation method according to claim 1 and 2, it is characterised in that the Nano-meter SiO_22Particle diameter be 10～100nm.
6. the preparation method according to claim 1 or 3, it is characterised in that the thickening agent is water-based thickener.
7. the preparation method according to claim 1 or 4, it is characterised in that the foaming agent is surfactant-based foaming
Agent.
8. preparation method according to claim 1, it is characterised in that the baking temperature in the step (3) is 45～55
DEG C, drying time is 10～14h.
9. a kind of sodium bicarbonate that in claim 1～8 prepared by preparation method described in any one, it is characterised in that the carbon
The size of sour hydrogen sodium is Nano grade.
10. sodium bicarbonate according to claim 9, it is characterised in that sodium bicarbonate structure in the form of sheets, size is：
Long 200～400nm, wide 60～100nm.
In a kind of 11. claim 1～8 in the sodium bicarbonate or claim 9～10 of preparation method preparation described in any one
Application of the sodium bicarbonate described in any one in expanded material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510979661.8A CN105540618B (en) | 2015-12-23 | 2015-12-23 | A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510979661.8A CN105540618B (en) | 2015-12-23 | 2015-12-23 | A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105540618A CN105540618A (en) | 2016-05-04 |
| CN105540618B true CN105540618B (en) | 2017-03-29 |
Family
ID=55820254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510979661.8A Expired - Fee Related CN105540618B (en) | 2015-12-23 | 2015-12-23 | A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105540618B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115744B (en) * | 2016-06-22 | 2017-12-01 | 湖南工业大学 | A kind of ultra-fine NaHCO3Particle and its preparation method and application |
| CN112694515A (en) * | 2021-01-20 | 2021-04-23 | 佳木斯冬梅大豆食品有限公司 | Deep processing method for extracting soybean protein peptide by membrane method |
| CN113636575B (en) * | 2021-08-13 | 2022-07-15 | 吉林省中研高分子材料股份有限公司 | Preparation of nano alkali metal carbonate and application thereof in preparation of poly (aryl ether ketone) |
| CN115092943A (en) * | 2022-03-03 | 2022-09-23 | 湖南银桥食品添加剂有限公司 | Preparation method of sodium bicarbonate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093588A (en) * | 2010-12-31 | 2011-06-15 | 常州市英特玛柯橡塑科技有限公司 | Composite foaming agent and preparation method and application thereof |
| WO2014096457A1 (en) * | 2012-12-21 | 2014-06-26 | Solvay Sa | Sodium bicarbonate particles manufactured by atomization |
| CN104244739A (en) * | 2012-02-20 | 2014-12-24 | 埃米内特有限公司 | Sodium bicarbonate product |
| CN104445217A (en) * | 2014-11-18 | 2015-03-25 | 北京科技大学 | Preparation method of nanopore SiO2 doped foaming cement |
-
2015
- 2015-12-23 CN CN201510979661.8A patent/CN105540618B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093588A (en) * | 2010-12-31 | 2011-06-15 | 常州市英特玛柯橡塑科技有限公司 | Composite foaming agent and preparation method and application thereof |
| CN104244739A (en) * | 2012-02-20 | 2014-12-24 | 埃米内特有限公司 | Sodium bicarbonate product |
| WO2014096457A1 (en) * | 2012-12-21 | 2014-06-26 | Solvay Sa | Sodium bicarbonate particles manufactured by atomization |
| CN104445217A (en) * | 2014-11-18 | 2015-03-25 | 北京科技大学 | Preparation method of nanopore SiO2 doped foaming cement |
Non-Patent Citations (1)
| Title |
|---|
| AC/NaHCO3复合发泡剂的改性及在PVB发泡材料中的应用研究;张国栋;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20131115;B016-12 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105540618A (en) | 2016-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105540618B (en) | A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material | |
| CN106495109B (en) | A kind of foam-like boron nitride block materials preparation method | |
| Yin et al. | Pickering emulsion: A novel template for microencapsulated phase change materials with polymer–silica hybrid shell | |
| CN103965470B (en) | Can the hydrophobically modified polymine whipping agent and its preparation method and application of release of carbon dioxide | |
| US8986838B2 (en) | Hollow carbon microparticle and method for producing same | |
| CN103205013B (en) | Polymer supercritical carbon dioxide foaming nucleating agent and preparation method and application thereof | |
| CN103224405B (en) | Method for preparing silicon nitride foam ceramic | |
| CN106747572A (en) | A kind of preparation method of carbon nanotube aerogel | |
| CN107365425B (en) | Preparation method and product of polyimide-based composite aerogel | |
| CN102924743A (en) | Method for preparing crystalline polyether-ether-ketone foam material | |
| Zhuang et al. | Preparation and characterisation of phenolic foam/HTAB-ATP nanocomposites | |
| CN114539623B (en) | Application of chitosan-based flame retardant in polyurethane | |
| CN105417569A (en) | Preparation method of rodlike nano-calcium carbonate | |
| CN105601979B (en) | A kind of preparation method of the phenol formaldehyde foam containing expanded graphite | |
| CN109825037A (en) | A kind of modified carbon nano-tube epoxy resin-base composite material | |
| CN102674379A (en) | Hollow mesoporous silicon dioxide nano particles and method for preparing same | |
| Wang et al. | Coaxial 3D printed anisotropic thermal conductive composite aerogel with aligned hierarchical porous carbon nanotubes and cellulose nanofibers | |
| CN110452480B (en) | Preparation method of ultra-light heat-insulating flexible aerogel | |
| CN104448394A (en) | Flame retardant having reactivity and adopting core-shell structure as well as preparation method and application of flame retardant | |
| CN103421198B (en) | Preparation method and application of low-temperature dissolving agar | |
| CN107365426B (en) | Polyimide-based composite aerogel and controllable preparation method and application thereof | |
| Wang et al. | Study of preparation and properties of fire-retardant melamine formaldehyde resin foam | |
| CN107684546A (en) | A kind of mesoporous silicon dioxide nano pharmaceutical carrier and preparation method thereof | |
| CN102863645B (en) | Method for preparing high-functionality foamed polymer material by supercritical CO2 | |
| CN103554893B (en) | A kind of composite flame-retardant agent for hard polyurethane foams |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170329 Termination date: 20181223 |