CN112300415A - Spherical nylon powder and preparation method and application thereof - Google Patents
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/122—Pulverisation by spraying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/88—Polyamides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/095—Oxygen containing compounds
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/11—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids from solid polymers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses spherical nylon powder and a preparation method and application thereof. The particle size of the spherical nylon powder is less than 10 mu m. The present invention replaces alcohol solvent of methanol and ethanol with organic acid, such as formic acid, and the nylon resin may be dissolved in formic acid at 100 deg.c and spray dried at higher temperature to produce spherical nylon powder with very small size, narrow size distribution, small apparent density and high dispersivity.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to spherical nylon powder and a preparation method and application thereof.
Background
Spherical nylon powder with ultra-fine particle size and narrow particle size distribution has smooth surface and very small apparent density, shows good sliding performance and unique soft feeling, can add high-quality touch feeling to cosmetics, and occupies more and more important position in the cosmetic industry.
The existing nylon powdering method mainly comprises a cryogenic grinding method, a solvent precipitation method and a polymerization method. The cryogenic grinding method is to utilize a grinder to cool and grind in liquid nitrogen, although the method has simple process, cryogenic equipment is needed, a large amount of cryogenic carriers are needed in the production process, the obtained particles obtained by grinding are irregular in shape, spherical particles are difficult to obtain, the particle size range is wide, and the requirements of cosmetics on powder appearance, flowability and the like are difficult to meet. The solvent precipitation method is to dissolve polyamide in a proper solvent and separate out powder by cooling crystallization. However, the existing common solvent precipitation method technology still cannot meet the requirements of cosmetics on powder morphology and ultrafine particle size. The polymerization method generally adopts methods similar to precipitation polymerization, emulsion polymerization and suspension polymerization to obtain nylon powder, the nylon powder obtained by the method is approximately spherical, the powder generally exists in micron-sized, the particle size is small, and the method can adapt to special requirements, but the process requirement is strict and large-scale industrial production is difficult.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of spherical nylon powder, which can prepare the spherical nylon powder with uniform, smooth, superfine particle size, narrow particle size distribution, small apparent density and good dispersibility.
The invention also provides spherical nylon powder and application of the spherical nylon powder.
The technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a preparation method of spherical nylon powder, which comprises the following steps:
dissolving nylon resin in organic acid to obtain nylon solution, and spray drying the nylon solution to obtain spherical nylon powder.
The preparation method of the spherical nylon powder at least has the following beneficial effects:
the invention replaces the alcohol solvent of methanol and ethanol with organic acid such as formic acid, the nylon resin can be dissolved in the formic acid at the temperature of not more than 100 ℃, compared with the alcohol solvent, the invention can lower the dissolving temperature of the nylon resin, avoid the risk brought by the high-temperature and high-pressure process of dissolving the nylon resin by alcohol, and has higher safety. Formic acid has a higher boiling point than alcohols and can be spray dried at a higher temperature. In the spray drying process, the atomized liquid drops are spherical under the action of surface tension, and the liquid drops are dried instantly when meeting hot air to keep the spherical shape, so that the spherical nylon powder with uniform, smooth, ultrafine particle size, narrow particle size distribution, small apparent density and good dispersibility is obtained, and the ultrahigh whiteness is kept. Meanwhile, formic acid is evaporated in the spray drying process and can be recycled after being condensed.
According to a preferred embodiment of the present invention, the organic acid comprises formic acid, and the temperature of the nylon resin dissolved in the formic acid is 80 to 100 ℃.
According to a preferred embodiment of the present invention, the mass ratio of the nylon resin to formic acid is 1: (15-30).
According to a more preferred embodiment of the present invention, the mass ratio of the nylon resin to formic acid is 1: (20-30).
According to a preferred embodiment of the invention, the diameter of the atomizing nozzle of the spray drying is 0.5-1.5 mm, the atomizing pressure is 0.1-0.5 MPa, the hot air inlet temperature is 150-200 ℃, and the hot air outlet temperature is 101-120 ℃.
According to a more preferable embodiment of the present invention, the spray drying has an atomizing nozzle diameter of 0.5 to 1mm, an atomizing pressure of 0.2 to 0.4Mpa, a hot air inlet temperature of 165 to 190 ℃, and a hot air outlet temperature of 101 to 110 ℃.
According to a preferred embodiment of the present invention, the spray drying is performed in a closed system, and both the hot air and the atomizing gas are inert gases, such as high-purity nitrogen.
According to a more preferred embodiment of the present invention, the nylon resin is at least one selected from the group consisting of nylon 6, nylon 610, nylon 11, nylon 12, nylon 1010, nylon 1012, and nylon 1212. Unless otherwise specified, all of the nylon resins are non-alcohol-soluble nylons.
According to a preferred embodiment of the present invention, the nylon solution further comprises the following steps after pressure spray drying: the spherical nylon powder was washed. A small amount of formic acid still remains on the surface of the spherical nylon powder after spray drying and needs to be washed and removed.
According to a preferred embodiment of the present invention, the spherical nylon powder is washed by adding the spherical nylon powder into an alcohol solvent, stirring and washing, and performing a second spray drying.
Formic acid remaining on the surface of the spherical powder is dissolved by using alcohols, and then the formic acid and the alcohols are removed by spray drying.
According to a preferred embodiment of the present invention, the stirring and washing temperature is 40 to 60 ℃.
According to a more preferred embodiment of the present invention, the agitation washing temperature is 40 to 50 ℃.
According to a preferred embodiment of the invention, the diameter of the atomizing nozzle of the second spray drying is 0.5-1.5 mm, the atomizing pressure is 0.1-0.5 MPa, the hot air inlet temperature is 150-200 ℃, and the hot air outlet temperature is 101-120 ℃.
According to a preferred embodiment of the invention, the diameter of the atomizing nozzle of the second spray drying is 0.75-1.2 mm, the atomizing pressure is 0.2-0.4 MPa, the hot air inlet temperature is 165-190 ℃, and the hot air outlet temperature is 101-110 ℃.
According to a preferred embodiment of the present invention, the alcoholic solvent is selected from the group consisting of general-purpose small molecular alcohols, such as methanol, ethanol, and the like.
The second aspect of the present invention is to provide a spherical nylon powder obtained according to the above method.
According to a preferred embodiment of the present invention, the spherical nylon powder has a particle size of 10 μm or less. The particle size of the nylon powder prepared by the traditional ethanol solvent method is more than 100 mu m, and the invention greatly reduces the particle size of the spherical nylon powder.
According to a more preferred embodiment of the present invention, the spherical nylon powder has an average particle diameter of 2 to 6 μm.
According to a preferred embodiment of the present invention, the spherical nylon powder has an apparent density of 150 to 210 g/L.
The third aspect of the present invention is to provide the use of the spherical nylon powder for the preparation of cosmetics.
Drawings
FIGS. 1 and 2 are scanning electron micrographs of the spherical nylon powder of example 1 at different magnifications.
FIG. 3 is a graph showing a distribution of particle diameters of spherical nylon powder of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples were all conventionally commercially available unless otherwise specified. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
A preparation method of spherical nylon powder comprises the following steps:
(1) 1kg of nylon 1012 granules and 25kg of formic acid are added into an enamel kettle, replaced by nitrogen, heated to 90 ℃ while stirring, and kept at the constant temperature for 90min to completely dissolve nylon, so as to obtain a clear and transparent nylon solution.
And (3) allowing the nylon solution to enter a pressure type spray dryer through a heat-preservation pipeline, and performing atomization drying granulation to obtain spherical nylon powder. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.75mm, the atomizing pressure is 0.4MPa, the hot air inlet temperature is 180 ℃, and the air outlet temperature is 102 ℃.
(2) Adding the spherical nylon powder prepared in the previous step and 20L of ethanol into an enamel kettle, replacing with nitrogen, heating to 45 ℃ while stirring, keeping the temperature for 60min, and drying by using a pressure type spray dryer to obtain a final powder product. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.75mm, the atomizing pressure is 0.4MPa, the hot air inlet temperature is 180 ℃, and the air outlet temperature is 102 ℃.
Scanning electron micrographs of the spherical nylon powder are shown in FIGS. 1 and 2, and the particle size distribution of the powder is shown in FIG. 3. As can be seen from FIGS. 1 and 2, the obtained spherical nylon powder has a regular spherical morphology and a smooth surface. Tests show that the spherical nylon powder has the average particle size of 2.5 microns, the maximum particle size of 6.8 microns, the apparent density of 180g/L and the whiteness of 92, and has the characteristics of ultra-small particle size, narrow particle size distribution, small apparent density, good dispersibility and the like.
Example 2
A preparation method of spherical nylon powder comprises the following steps:
(1) adding 1kg of nylon 12 granules and 28kg of formic acid into an enamel kettle, replacing with nitrogen, heating to 90 ℃ while stirring, and keeping the temperature for 90min to completely dissolve nylon to obtain a clear and transparent nylon solution.
And (3) allowing the nylon solution to enter a pressure type spray dryer through a heat-preservation pipeline, and performing atomization drying granulation to obtain spherical nylon powder. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.5mm, the atomizing pressure is 0.4MPa, the hot air inlet temperature is 180 ℃, and the air outlet temperature is 102 ℃.
(2) Adding the spherical nylon powder prepared in the previous step and 20L of ethanol into an enamel kettle, replacing with nitrogen, heating to 45 ℃ while stirring, keeping the temperature for 60min, and drying by using a pressure type spray dryer to obtain a final powder product. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.5mm, the atomizing pressure is 0.4MPa, the hot air inlet temperature is 180 ℃, and the air outlet temperature is 102 ℃.
The spherical nylon powder was tested to have an average particle size of 2.7 μm, a maximum particle size of 5.6 μm, an apparent density of 153g/L and a whiteness of 94.
Example 3
A preparation method of spherical nylon powder comprises the following steps:
(1) adding 1kg of nylon 610 granules and 30kg of formic acid into an enamel kettle, replacing with nitrogen, heating to 90 ℃ while stirring, and keeping the temperature for 120min to completely dissolve nylon to obtain a clear and transparent nylon solution.
And (3) allowing the nylon solution to enter a pressure type spray dryer through a heat-preservation pipeline, and performing atomization drying granulation to obtain spherical nylon powder. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.75mm, the atomizing pressure is 0.5MPa, the hot air inlet temperature is 185 ℃, and the air outlet temperature is 102 ℃.
(2) Adding the spherical nylon powder prepared in the previous step and 20L of ethanol into an enamel kettle, replacing with nitrogen, heating to 45 ℃ while stirring, keeping the temperature for 60min, and drying by using a pressure type spray dryer to obtain a final powder product. The pressure type spray dryer is a closed system, hot air is high-purity nitrogen, the diameter of an atomizing nozzle is 0.75mm, the atomizing pressure is 0.5MPa, the hot air inlet temperature is 185 ℃, and the air outlet temperature is 102 ℃.
The spherical nylon powder was tested to have an average particle size of 5.4 μm, a maximum particle size of 9.7 μm, an apparent density of 204g/L, and a whiteness of 91.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of spherical nylon powder is characterized in that: the method comprises the following steps:
dissolving nylon resin in organic acid to obtain nylon solution, and spray drying the nylon solution to obtain spherical nylon powder.
2. The method for preparing spherical nylon powder according to claim 1, wherein: the organic acid comprises formic acid, and the temperature for dissolving the nylon resin in the formic acid is 80-100 ℃.
3. The method for preparing spherical nylon powder according to claim 1, wherein: the mass ratio of the nylon resin to formic acid is 1: (15-30).
4. The method for preparing spherical nylon powder according to claim 1, wherein: the hot air inlet temperature of the spray drying is 150-200 ℃, and the hot air outlet temperature is 101-120 ℃.
5. The method for producing spherical nylon powder according to any one of claims 1 to 4, characterized in that: the nylon solution further comprises the following steps after pressure type spray drying: the spherical nylon powder was washed.
6. The method for preparing spherical nylon powder according to claim 5, wherein: the method for washing the spherical nylon powder comprises the steps of adding the spherical nylon powder into an alcohol solvent, stirring and washing, and carrying out secondary spray drying.
7. A spherical nylon powder obtained by the production method according to any one of claims 1 to 6.
8. The spherical nylon powder according to claim 7, wherein: the particle size of the spherical nylon powder is less than 10 mu m.
9. The spherical nylon powder according to claim 7, wherein: the apparent density of the spherical nylon powder is 150-210 g/L.
10. Use of the spherical nylon powder according to any one of claims 7 to 9 for the preparation of cosmetics.
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Application publication date: 20210202 |