CN111471319B - Preparation method of pore-foaming agent - Google Patents
Preparation method of pore-foaming agent Download PDFInfo
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- CN111471319B CN111471319B CN202010450124.5A CN202010450124A CN111471319B CN 111471319 B CN111471319 B CN 111471319B CN 202010450124 A CN202010450124 A CN 202010450124A CN 111471319 B CN111471319 B CN 111471319B
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- calcium carbonate
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- 239000004088 foaming agent Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 126
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 63
- 239000000843 powder Substances 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000000227 grinding Methods 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000077 silane Inorganic materials 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 229910052613 tourmaline Inorganic materials 0.000 claims description 42
- 229940070527 tourmaline Drugs 0.000 claims description 42
- 239000011032 tourmaline Substances 0.000 claims description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000003361 porogen Substances 0.000 claims description 16
- 235000021355 Stearic acid Nutrition 0.000 claims description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 13
- 239000008117 stearic acid Substances 0.000 claims description 13
- LXXKJGXDEZDJOM-UHFFFAOYSA-N [Fe].[Mg].[Ca] Chemical compound [Fe].[Mg].[Ca] LXXKJGXDEZDJOM-UHFFFAOYSA-N 0.000 claims description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 9
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 8
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 8
- 239000010954 inorganic particle Substances 0.000 claims description 8
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 6
- 238000009775 high-speed stirring Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000001914 filtration Methods 0.000 description 14
- 239000006087 Silane Coupling Agent Substances 0.000 description 11
- 239000011148 porous material Substances 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000002904 solvent Substances 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 239000008280 blood Substances 0.000 description 5
- 210000004369 blood Anatomy 0.000 description 5
- 230000035515 penetration Effects 0.000 description 5
- 230000029058 respiratory gaseous exchange Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 stearic acid modified iron-calcium-magnesium Chemical class 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005686 electrostatic field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 210000005260 human cell Anatomy 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
- C09C1/022—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
- C09C1/022—Treatment with inorganic compounds
- C09C1/024—Coating
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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Abstract
The invention discloses a preparation method of a pore-foaming agent, which comprises the following steps: (1) grinding high-mesh calcium carbonate powder by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed silane solution, grinding for 60-600min, and performing filter pressing and drying to prepare wet activated ground calcium carbonate powder; (2) stirring the wet-process activated ground calcium carbonate powder at a high speed at 80 ℃, adding a coating material with the mass fraction of 0.01-5%, heating to 120 ℃, and continuing stirring for 60min to prepare coated calcium carbonate powder; (3) adding inorganic grinding aid particles and coated calcium carbonate powder into a stirring mill at the same time, and grinding for 60-600min at normal temperature; (4) and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent for the breathable film of the medical care product. The invention has the beneficial effects that: (1) the hole making effect is uniform; (2) functionalizing a pore-foaming agent; (3) the process is simple and the preparation efficiency is high.
Description
Technical Field
The invention relates to the technical field of production of pore-foaming agents, in particular to a preparation method of a pore-foaming agent.
Background
The breathable film is a film prepared by casting or blow molding resin filled with superfine calcium carbonate powder, and then the film is subjected to unidirectional or bidirectional stretching to cause the debonding of a calcium carbonate/resin interface to generate micro-nano holes, so that the breathable film has the functions of ventilation (steam), water resistance (liquid, bacteria and dust), and is widely applied to the fields of medical protective clothing, the outer layer (waterproof layer) and the inner layer (water absorption layer) of a mask, hygienic products and the like. The superfine calcium carbonate plays a role of a pore-forming agent, the particle size and the distribution width of the superfine calcium carbonate, and the surface characteristics determine the pore-forming effect of the breathable film, so that the breathable and water-blocking capability of the product is influenced.
According to the forecast of market research company MarketsandMarkets, the annual growth rate of the global breathable film market in 2016-2024 years is kept above 8.5%, and the global breathable film market is expected to reach about $ 400 billion by 2024 years. China is the country with the most production and application of breathable films in the world, according to statistics of the national statistical bureau, the yield of the breathable films in 2018 accounts for about 25% of the total yield of plastic products, the breathable films are increased at a speed of about 9%, and the breathable films are one of the categories of the plastic products with the fastest yield increase. In 2018, 65 enterprises with the breathable film yield of more than 5000 tons exist in China, and the ultrafine calcium carbonate powder is used as an important raw material of the breathable film, so that the position importance and the future market prospect are very wide.
Therefore, under the background of rapid development of the current domestic breathable film market, basic research of key technologies of industrialization of the special pore-forming agent for the breathable film is developed, the pore-forming capability and rich functionality of the pore-forming agent are optimized, monopoly and technical blockade of foreign/foreign enterprises on related production process technologies is broken, and the importance and the necessity of protecting the safety of domestic raw materials are self-evident.
Disclosure of Invention
The invention aims to provide a preparation method of a pore-foaming agent, aiming at solving the defects in the prior art, the modified tourmaline can be coated on the surface of calcium carbonate powder based on mechanical occlusion force and intermolecular force, so that pores are formed on a tourmaline/calcium carbonate powder interface, the pore-forming capability is improved, and the pores have the functions of sterilization and negative ion release. The problems of weak hole making capability and functional loss of the hole making agent in the prior art are solved.
The invention provides a preparation method of a pore-foaming agent, which comprises the following steps:
(1) and (3) wet activation grinding: grinding high-mesh calcium carbonate powder by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed silane solution, grinding for 60-600min, and performing filter pressing and drying to prepare wet activated ground calcium carbonate powder;
(2) and (3) dry coating: high-speed stirring the ground calcium carbonate powder by a wet method at 80 ℃, adding a coating material with the mass fraction of 0.01-5%, heating to 120 ℃, and continuously stirring for 60min to prepare the coated calcium carbonate powder;
(3) grinding and coating inorganic particles: adding inorganic grinding aid particles and coated calcium carbonate powder into a stirring mill at the same time, and grinding for 60-600min at normal temperature;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent for the breathable film of the medical care product.
In the method for preparing a porogen, it is preferable that the hydrolyzed silane solution in step (1) is prepared from a silane coupling agent, a pH regulator and a solvent.
A method of preparing a porogen as described above, wherein preferably the silane coupling agent is gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
In the method for preparing a porogen, the pH regulator is preferably ammonia water, and the pH is preferably adjusted to 9.
A method for preparing a porogen as described above, wherein preferably the solvent is an aqueous ethanol solution.
The preparation method of the porogen as described above, wherein preferably, the mixture ratio of the hydrolyzed silane solution by weight is: 0.1-20% of silane coupling agent, 1-20% of PH regulator and the balance of solvent.
The method for preparing a porogen as described above, wherein preferably, the coating material in step (2) is at least one of oleamide, PE wax and PP wax.
The method for preparing a porogen as described above, wherein preferably, in step (3), the inorganic grinding-aid particles are at least one of iron-calcium-magnesium tourmaline, calcium-magnesium tourmaline and alkali-free iron tourmaline, the particle size is less than 100nm, and the surface is coated with a layer of stearic acid molecules.
The method for preparing a porogen as described above, wherein the iron-calcium-magnesium tourmaline, calcium-magnesium tourmaline and alkali-free iron tourmaline preferably have a density 15% greater than that of calcium carbonate and a Mohs hardness of 8.
Compared with the prior art, the invention has the beneficial effects that: (1) the hole making effect is uniform: the pore-making agent prepared by the invention is calcium carbonate powder wrapped by tourmaline, and because the tourmaline has a permanent spontaneous electrode and generates an electrostatic field, the tourmaline can be separated by adopting an electrostatic classification process, so that the separation efficiency and the separation precision are improved. In the preparation process of the breathable film, the processing flowability of the pore-forming agent is directly influenced by the particle size and the distribution of the pore-forming agent, so that the production speed and the process stability of the breathable film are determined, and the stretching pore-forming property, the pore structure, the air permeability and the mechanical property of the breathable film are also greatly influenced. Therefore, the pore-forming agent prepared by the invention has uniform pore-forming effect. The invention makes tourmaline coated on the surface of calcium carbonate by designing mechanical bite force (formed in a stirring mill) and intermolecular force (both of which are oleophylic coating), so that the binding force of the tourmaline/calcium carbonate interface is weak, and the difficulty of hole making is reduced. (2) Pore-foaming agent functionalization: according to the invention, the tourmaline/calcium carbonate interface is debonded to form a microporous structure in the process of hole making by using the prepared hole making agent, and the tourmaline is positioned on the inner surface of the hole, so that on one hand, tourmaline can generate an electrostatic field and release negative ions to achieve the sterilization function; in addition, the tourmaline can emit far infrared rays with the wavelength of 4-14um and the emissivity of more than 0.92 at normal temperature, so as to stimulate the activity of human cells, promote the blood circulation and metabolism of human bodies and improve the wearing comfort of the medical care product. (3) Simple process and high preparation efficiency: according to the project, the modified tourmaline and the calcium carbonate powder are added in the stirring mill at the same time, so that the high-hardness tourmaline plays a role of grinding aid in the stirring process, and the crushing efficiency of the calcium carbonate powder is improved; in addition, reverse dissociation of mineral is performed in the crushing processExposing the unsaturated particle Ca2+And CO3 2-And Ca2+And CO3 2-The particles have high unsaturation degree and strong activity, and the tourmaline with a spontaneous electrode is adsorbed on the surfaces of the active sites, so that the source kinetic energy of secondary agglomeration is thoroughly eliminated, the heat accumulation and the electrostatic attraction are eliminated, and the stable and durable dispersibility and flowability are effectively ensured.
Drawings
FIG. 1 is a schematic structural diagram of a porogen prepared by the method of example 1 of this invention;
FIG. 2 is a schematic structural diagram of a breathable film made of a porogen prepared by the method of example 1.
Detailed Description
The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.
The invention provides a preparation method of a pore-foaming agent, which comprises the following steps:
(1) and (3) wet activation grinding: grinding high-mesh calcium carbonate powder by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed silane solution, grinding for 60-600min, and performing filter pressing and drying to prepare wet activated ground calcium carbonate powder;
(2) and (3) dry coating: high-speed stirring the ground calcium carbonate powder by a wet method at 80 ℃, adding a coating material with the mass fraction of 0.01-5%, heating to 120 ℃, and continuously stirring for 60min to prepare the coated calcium carbonate powder;
(3) grinding and coating inorganic particles: adding inorganic grinding aid particles and coated calcium carbonate powder into a stirring mill at the same time, and grinding for 60-600min at normal temperature;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent for the breathable film of the medical care product.
The hydrolyzed silane solution in the step (1) is prepared from a silane coupling agent, a pH regulator and a solvent.
The silane coupling agent is gamma- (2, 3-glycidoxy) propyl trimethoxy silane.
The pH regulator is ammonia water, and the pH is regulated to 9.
The solvent is an aqueous ethanol solution.
The hydrolyzed silane solution comprises the following components in parts by weight: 0.1-20% of silane coupling agent, 1-20% of PH regulator and the balance of solvent.
In the step (2), the coating material is at least one of oleamide, PE wax and PP wax.
In the step (3), the inorganic grinding-aid particles are at least one of iron-calcium-magnesium tourmaline, calcium-magnesium tourmaline and alkali-free iron tourmaline, the particle size is less than 100nm, and a layer of stearic acid molecules is coated on the surface of the inorganic grinding-aid particles.
The density of the iron calcium magnesium tourmaline, the calcium magnesium tourmaline and the alkali-free iron tourmaline is 15 percent higher than that of calcium carbonate, and the Mohs hardness is 8.
Example 1 of the invention:
a preparation method of a pore-foaming agent comprises the following steps:
(1) and (3) wet activation grinding: grinding calcium carbonate powder to 600 meshes by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane solution (the mass ratio of a silane coupling agent to water to ethanol is 0.1:20:79.9), continuously grinding for 60min, and preparing wet activated ground calcium carbonate powder after press filtration and drying;
(2) and (3) dry coating: stirring at high speed at 80 ℃ to activate the ground calcium carbonate powder by a wet method, adding 0.01 percent of oleamide by mass, heating to 120 ℃, and continuing stirring for 60min to prepare coated calcium carbonate powder;
(3) grinding and coating inorganic particles: placing the coated calcium carbonate powder and the stearic acid modified iron-calcium-magnesium tourmaline into a stirring mill, and grinding for 600min at normal temperature;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent for the breathable film of the medical care product.
The parameters of the porogen prepared by the method of this example are as follows: median particle diameter (D)50) At 1.8 μm, 97% particle size (D)97)5 mu m, 10 particles of 1-5 mu m% of particles having a particle diameter of 10 μm or more is 90ppm, and BET specific surface area is 10m2G, density of 3g/cm3。
As shown in fig. 1, the pore-forming agent prepared by the method of this embodiment has a covalent bond of calcium carbonate/silane interface force, a covalent bond of iron calcium magnesium tourmaline/stearic acid interface force, and an intermolecular force of stearic acid/oleamide/silane interface force.
In the stretching process of the breathable film prepared by adopting the pore-forming agent, because the acting force of a stearic acid/oleamide/silane interface is smaller than that of an iron-calcium-magnesium tourmaline/stearic acid interface and that of a calcium carbonate/silane interface, the stearic acid/oleamide/silane interface is cracked, so that the iron-calcium-magnesium tourmaline is positioned on the inner surface of a pore (as shown in figure 2), the performance of the breathable film is as shown in the following table 1 (the test method is shown in EN14126-2003 standard), and the breathable film is comfortable to wear by medical workers.
TABLE 1 breathable film Properties
| Details of the indicators | Numerical value |
| Bacterial filtration efficiency | 98.5％ |
| Non-oily particle filtration efficiency | 98.5％ |
| Synthetic blood penetration | 160mmHg |
| Resistance to breathing | 5.5mm H2O/cm2 |
| Amount of negative ion released | 600 pieces/cm3 |
| Average pore diameter of breathable film | 5μm |
Example 2 of the invention:
a preparation method of a pore-foaming agent comprises the following steps:
(1) and (3) wet activation grinding: grinding calcium carbonate powder to 600 meshes by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane solution (the mass ratio of a silane coupling agent to water to ethanol is 20:0.1:79.9), continuously grinding for 600min, and preparing wet activated ground calcium carbonate powder after press filtration and drying;
(2) and (3) dry coating: stirring the ground calcium carbonate powder at a high speed at 80 ℃ by a wet method, adding 5% by mass of PE wax, heating to 120 ℃, and continuing stirring for 60min to prepare coated calcium carbonate powder;
(3) grinding and coating inorganic particles: placing calcium carbonate powder and stearic acid modified alkali-free iron tourmaline in a stirring mill, and grinding for 100min at normal temperature;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent special for the breathable film of the medical care product.
The parameters of the porogen prepared by the method of this example are as follows: d50At 1.8 to 2.2 μm, D97Less than 6.5 μm, more than 60% of particles with the diameter of 1-5 μm, less than 100ppm of particles with the diameter of more than 10 μm, and BET specific surface area of 5-15m2G, density>2.9g/cm3. Namely, the pore-forming agent special for the breathable film of the medical care product is prepared.
The performance of the breathable film prepared by adopting the pore-foaming agent is shown in the following table 2, and the breathable film is comfortable to wear by medical workers.
TABLE 2 breathable film Properties
| Details of the indicators | Numerical value |
| Bacterial filtration efficiency | 98.1％ |
| Non-oily particle filtration efficiency | 98.1％ |
| Synthetic blood penetration | 80mmHg |
| Resistance to breathing | 3.5mm H2O/cm2 |
| Amount of negative ion released | 800 pieces/cm3 |
| Average pore diameter of breathable film | 8μm |
Example 3 of the invention:
a preparation method of a pore-foaming agent comprises the following steps:
(1) and (3) wet activation grinding: grinding calcium carbonate powder to 600 meshes by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane solution (the mass ratio of a silane coupling agent to water to ethanol is 1:19:80), continuously grinding for 400min, and performing filter pressing and drying to prepare wet activated ground calcium carbonate powder;
(2) and (3) dry coating: stirring the ground calcium carbonate powder at a high speed at 80 ℃ by a wet method, adding 3% by mass of PP wax, heating to 120 ℃, and continuously stirring for 60min to prepare coated calcium carbonate powder;
(3) grinding and coating inorganic particles: placing the coated calcium carbonate powder and the stearic acid modified calcium-magnesium tourmaline into a stirring mill, and grinding for 100min at normal temperature;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent special for the breathable film of the medical care product.
The parameters of the porogen prepared by the method of this example are as follows: d50At 1.8 μm, D975 μm, particles of 1-5 μm accounting for 67%, particles more than 10 μm less than 95ppm, and BET specific surface area of 12m2G, density of 2.99g/cm3. Namely, the pore-forming agent special for the breathable film of the medical care product is prepared.
The performance of the breathable film prepared by adopting the pore-foaming agent is shown in the following table 3, and the breathable film is comfortable to wear by medical workers.
TABLE 3 breathable film Properties
| Details of the indicators | Numerical value |
| Bacterial filtration efficiency | 99％ |
| Non-oily particle filtration efficiency | 99％ |
| Synthetic blood penetration | 80mmHg |
| Resistance to breathing | 3.0mm H2O/cm2 |
| Amount of negative ion released | 800 pieces/cm3 |
| Average pore diameter of breathable film | 3μm |
Example 4 of the invention:
a preparation method of a pore-foaming agent comprises the following steps:
(1) and (3) wet activation grinding: grinding calcium carbonate powder to 600 meshes by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane solution (the mass ratio of a silane coupling agent to water to ethanol is 0.1:20:79.9), continuously grinding for 100min, and preparing wet activated ground calcium carbonate powder after press filtration and drying;
(2) and (3) dry coating: stirring the ground calcium carbonate powder at a high speed at 80 ℃ by a wet method, adding 1% by mass of oleamide, PE wax and PP wax, heating to 120 ℃, and continuing stirring for 60min to prepare coated calcium carbonate powder;
(3) grinding and coating inorganic particles: placing the coated calcium carbonate powder, stearic acid modified iron calcium magnesium tourmaline, calcium magnesium tourmaline and alkali-free ferrum and gas in a stirring mill, and grinding at normal temperature for 60-600 min;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent special for the breathable film of the medical care product.
The parameters of the porogen prepared by the method of this example are as follows: d50Is 2.2 μm, D974 μm, particles of 1-5 μm accounting for 70%, particles more than 10 μm less than 80ppm, and BET specific surface area of 15m2G, density 3.02g/cm3. Namely, the pore-forming agent special for the breathable film of the medical care product is prepared.
The properties of the breathable film prepared by using the pore-foaming agent are shown in the following table 4, and the breathable film is comfortable to wear by medical workers.
TABLE 4 breathable film Properties
| Details of the indicators | Numerical value |
| Bacterial filtration efficiency | 98％ |
| Non-oily particle filtration efficiency | 98％ |
| Synthetic blood penetration | 80mmHg |
| Resistance to breathing | 2.0mm H2O/cm2 |
| Amount of negative ion released | 800 pieces/cm3 |
| Average pore diameter of breathable film | 6μm |
Example 5 of the invention:
a preparation method of a pore-foaming agent comprises the following steps:
(1) and (3) wet activation grinding: grinding calcium carbonate powder to 600 meshes by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane solution (the mass ratio of a silane coupling agent to water to ethanol is 0.1:20:79.9), continuously grinding for 130min, and preparing wet activated ground calcium carbonate powder after press filtration and drying;
(2) and (3) dry coating: high-speed stirring the ground calcium carbonate powder at 80 ℃, adding 2 mass percent of oleic acid amide, PE wax and PP wax, heating to 120 ℃, and continuously stirring for 60min to prepare coated calcium carbonate powder;
(3) grinding and coating inorganic particles: placing the coated calcium carbonate powder, stearic acid modified iron calcium magnesium tourmaline, calcium magnesium tourmaline and alkali-free ferrum and gas in a stirring mill, and grinding at normal temperature for 60-600 min;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent special for the breathable film of the medical care product.
The parameters of the porogen prepared by the method of this example are as follows: d50Is 2.1 μm, D975 μm, particles of 1-5 μm accounting for 65%, more than 10 μm particles less than 90ppm, and BET specific surface area of 10m2G, density 3.05g/cm3. Namely, the pore-forming agent special for the breathable film of the medical care product is prepared.
The performance of the breathable film prepared by adopting the pore-foaming agent is shown in the following table 5, and the breathable film is comfortable to wear by medical workers.
TABLE 5 breathable film Properties
| Details of the indicators | Numerical value |
| Bacterial filtration efficiency | 99 |
| Non-oily particle filtration efficiency | 98 |
| Synthetic blood penetration | 80mmHg |
| Resistance to breathing | 3.0mm H2O/cm2 |
| Amount of negative ion released | 800 pieces/cm3 |
| Average pore diameter of breathable film | 5μm |
The construction, features and functions of the present invention are described in detail in the embodiments illustrated in the drawings, which are only preferred embodiments of the present invention, but the present invention is not limited by the drawings, and all equivalent embodiments modified or changed according to the idea of the present invention should fall within the protection scope of the present invention without departing from the spirit of the present invention covered by the description and the drawings.
Claims (2)
1. A preparation method of a pore-foaming agent is characterized by comprising the following steps: the method comprises the following steps:
(1) and (3) wet activation grinding: grinding high-mesh calcium carbonate powder by adopting a wet ball milling process, wherein the system temperature is 80 ℃, adding a hydrolyzed silane solution, grinding for 60-600min, and performing filter pressing and drying to prepare wet activated ground calcium carbonate powder; the silane solution is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane;
(2) and (3) dry coating: high-speed stirring the ground calcium carbonate powder by a wet method at 80 ℃, adding a coating material with the mass fraction of 0.01-5%, heating to 120 ℃, and continuously stirring for 60min to prepare the coated calcium carbonate powder; the coating material is at least one of oleamide, PE wax and PP wax;
(3) grinding and coating inorganic particles: adding inorganic grinding aid particles and coated calcium carbonate powder into a stirring mill at the same time, and grinding for 60-600min at normal temperature; the inorganic grinding-aid particles are at least one of iron-calcium-magnesium tourmaline, calcium-magnesium tourmaline and alkali-free iron tourmaline, the particle size is less than 100nm, and a layer of stearic acid molecules is coated on the surface of the inorganic grinding-aid particles;
(4) fine grading: and (4) selecting the powder separated in the step (3) by an electrostatic classification process to prepare the pore-foaming agent for the breathable film of the medical care product.
2. The method for preparing a porogen according to claim 1, characterized in that: the density of the iron calcium magnesium tourmaline, the calcium magnesium tourmaline and the alkali-free iron tourmaline is 15 percent higher than that of calcium carbonate, and the Mohs hardness is 8.
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| KR100718499B1 (en) * | 2006-09-14 | 2007-05-18 | 김동현 | Eco-friendly elastic chip manufacturing method using steel slag or sand and silica sand and eco-friendly permeable flooring material |
| CN102391690A (en) * | 2011-08-05 | 2012-03-28 | 江西理工大学 | High whiteness tourmaline negative ion powder and coating process |
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| CN111073346A (en) * | 2019-11-14 | 2020-04-28 | 江西广源化工有限责任公司 | Preparation method of wet ball-milling modified calcium carbonate powder special for water-based polyurethane wood lacquer primer |
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| KR100718499B1 (en) * | 2006-09-14 | 2007-05-18 | 김동현 | Eco-friendly elastic chip manufacturing method using steel slag or sand and silica sand and eco-friendly permeable flooring material |
| CN102391690A (en) * | 2011-08-05 | 2012-03-28 | 江西理工大学 | High whiteness tourmaline negative ion powder and coating process |
| CN102675918A (en) * | 2012-05-04 | 2012-09-19 | 安徽江东科技粉业有限公司 | Preparation method of low-yellowness antibacterial calcium carbonate functional composite powder for ventilated membrane |
| CN111073346A (en) * | 2019-11-14 | 2020-04-28 | 江西广源化工有限责任公司 | Preparation method of wet ball-milling modified calcium carbonate powder special for water-based polyurethane wood lacquer primer |
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Effective date of registration: 20231109 Address after: 242500 Yunling Economic Development Zone, Jing County, Xuancheng City, Anhui Province Patentee after: ANHUI JIANGDONG TECHNOLOGY POWDER INDUSTRY Co.,Ltd. Address before: No.99 Jinxiu Avenue, Hefei Economic Development Zone, Anhui Province 230601 Patentee before: HEFEI University |