CN112850723A - Preparation method of functional group modified aerogel particles for spinning and fiber spinning - Google Patents
Preparation method of functional group modified aerogel particles for spinning and fiber spinning Download PDFInfo
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Abstract
The invention provides a preparation method of functional group modified aerogel particles for spinning and fiber spinning, which is prepared by the following steps: (1) a mixing step, (2) a hydrolysis step, (3) a condensation dispersion step, (4) a further surface functional group modification step, and (5) a solvent evaporation drying step. The invention can be used for producing the surface functional group modified aerogel powder continuously or in batch, and the manufacturing process is simple and the manufacturing speed is high. The functional modified aerogel powder can obviously improve excellent acting force between the functional modified aerogel powder and various plastics, improve the composite mixing efficiency between the aerogel and the plastics, and improve the dispersion of the functional modified aerogel powder in the plastics so as to improve the functionality of an aerogel composite material and the spinnability of subsequent fiber spinning.
Description
Technical Field
The invention relates to a preparation method of functional group modified aerogel particles for spinning and fiber spinning, in particular to a continuous process combining various functional group modifying agents and an aerogel sol-gel synthesis technology to improve the application property and the production speed of functional group modified aerogel powder. The invention relates to a method for improving the spinning property of aerogel composite fiber, improving the usability of aerogel applied to textile post-processing and the functional modified aerogel powder, which is characterized in that a special functional group is added in the aerogel and on the surface of the aerogel to increase the bonding force of the aerogel powder and a post-processing base material such as plastic or an adhesive and promote the addition of the functional modified aerogel powder in the base material such as plastic and post-processing colloid and the characteristic that the functional modified aerogel powder can be uniformly dispersed in the base material is improved.
Background
Aerogel is a porous material with a three-dimensional net structure, has a scientific and technological product with low density, high specific surface area and low thermal conductivity, and is mainly applied to heat insulation materials at present. Since the aerogel powder has an extremely low bulk density (about 0.04-0.2 g/cm)3) And relative to the density of the subsequently processed plastic material (0.8-1.35 g/cm)3) Because the density difference between the aerogel and the aerogel is large and the specific volume of the aerogel is extremely large, the addition amount of the aerogel needs to be increased to achieve effective functionality in order to achieve the application of the aerogel in textile or spinning industry; such as light weight, high thermal insulation, high fire resistance, and low dripping. Large amounts of aerogel must therefore be added to the organic plastic. However, the aerogel technology produced on the market only provides hydrophobic modified aerogel powder, but the chemical structure of the hydrophobic modified aerogel powder is not matched with the chemical structure of a plastic substrate applied to textile industry such as spinning. Therefore, the currently commercialized aerogel powder has poor workability in blending with plastics, is not added in sufficient amount and easily aggregates inside plastics, resulting in spinning processEasily broken filaments and the like. Particularly, high-pressure dust is very easily generated when the aerogel powder is blended with plastic under high-temperature conditions, thereby limiting the applicability of the aerogel powder in a spinning or spinning process. In order to solve the problems, the patent discloses a continuous production technology combining an improved gel-melt adhesive synthesis technology with subsequent surface modification, so that aerogel is subjected to continuous liquid phase surface modification to produce aerogel powder suitable for spinning and textile post-processing application. In order to increase the effective modifying effect of the aerogel, the invention uses a continuous two-step modifying technology; the front-stage hydrolysis modification and the rear-stage aging surface modification promote the effective modification of aerogel powder to promote the acting force between the aerogel powder and the plastic base material so as to improve the addition and dispersion properties. In the post-processing process of the aerogel powder, the structure of the aerogel powder is very fragile, so the aerogel powder is easy to break under the action of processing shear stress when the aerogel powder is mixed with plastics under a high-temperature condition, and the modification effect is not good when the surface of the aerogel powder is modified only by crushing, so that the continuous two-step modification technology is carried out to ensure that the aerogel powder obtains effective modification of the interior of particles and the surface of the particles.
The traditional aerogel preparing method is sol-gel synthesis, which is mainly to mix precursors such as silicon alkoxides (alkoxysilanes), methyl orthosilicate or water glass and the like with an organic solvent, and then to add an acid catalyst into the mixture by a two-step method to perform hydrolysis reaction (hydrosis). After the hydrolysis reaction is carried out for a certain period of time, an alkali catalyst is added to carry out condensation reaction (condensation), and sol is gradually formed in the condensation reaction process. Molecules in the sol are continuously subjected to condensation reaction bonding to gradually form semi-solid polymer gel, and the sol is cured (formed) for a period of time to form a stable three-dimensional network structure. And finally, extracting and drying the solvents such as water, methanol and the like in the aerogel system by using a supercritical drying technology to obtain porous dry aerogel powder.
In addition, the preparation method of the hydrophobic aerogel is a sol-gel synthesis method, which mainly comprises the steps of mixing precursors such as methyl silicon alkoxide (alkoxy silanes) such as MTMS or MTES and the like with an organic solvent, and then adding an alkali catalyst into the mixture by a one-step method to perform hydrolysis reaction (hydrosis). After the hydrolysis reaction is carried out for a certain period of time, condensation reaction (condensation) is carried out, and sol is gradually formed in the condensation reaction process. Molecules in the sol are continuously subjected to condensation reaction bonding to gradually form semisolid polymer gel, and then the solvent is replaced by Isopropanol (IPA) or Ethanol (EA) for two to three days under the aging (aging) for a period of time, so that the hydrophobic sol forms a stable three-dimensional network structure. And finally, drying the solvents such as ethanol or isopropanol and the like in the aerogel system by using a normal pressure drying technology to obtain the porous dry aerogel block.
Because the drying technology adopted by the preparation method of the aerogel is a supercritical drying technology or utilizes a plurality of times of solvent replacement for two to three days, the aerogel can be prevented from being cracked due to the influence of the surface tension of water in the normal pressure drying process. However, because the supercritical drying technology is carried out under high pressure, the method is only suitable for drying a very small amount of aerogel; the solvent replacement is time-consuming in the night, which is not beneficial to mass production and reduces the production cost of the aerogel.
On the other hand, commercial aerogels are mainly hydrophobic aerogel powders, which are only dispersible in oil-soluble systems in use, but not in water-soluble system solutions. In addition, the current commercial blending process of hydrophobic aerogel powder and plastic often results in uneven blending or no mixing in large quantities, which is mainly caused by the fact that the surface properties of the aerogel are not matched with the plastic, thus the aerogel cannot be uniformly dispersed in the plastic.
In other related prior art, such as taiwan patent publication No. 200835648, "porous material and method for preparing the same", the porous material is prepared by synthesizing silicon alkoxides (such as TEOS) or silicate compounds (such as water glass) and an organic solvent by a sol-gel method, and modifying the synthesized material with a modifier, so that hydrophilic functional groups on the surface of the porous material are replaced with hydrophobic functional groups, and the aerogel can be prevented from being broken due to the influence of surface tension of moisture, and thus can be dried at room temperature and normal pressure.
The prior art uses the normal temperature and pressure multi-gradient solvent replacement technology for the hydrophobic modification of the aerogel, but the hydrophobic modification process needs to be carried out for more than 24 hours under the normal temperature and pressure condition, the time required by the process is too long, and the process is not cost-effective.
Another related prior art, such as taiwan patent publication No. 201728273, "synthetic fiber containing aerogel and polymer material, manufacturing method thereof, and article containing the same", mainly describes a composite fiber containing polymer material and aerogel particles, a product containing the same, and a method for forming the same, wherein the composite fiber is formed by blending a general hydrophobic aerogel powder and a plastic ester material, the aerogel powder has a particle size of 0.3 μm to 20 μm, and the aerogel concentration is 2 vol.% to 70 vol.%.
The prior art proposes that the synthetic fiber containing aerogel and polymer material is only a concept of adding general aerogel powder into the synthetic fiber, but the surface hydrophobicity modification of the hydrophobic aerogel powder in the market at present mainly comprises that silicon alkoxides (such as TEOS) are hydrolyzed and then condensed and aggregated to form an aerogel block, and then the aerogel block is crushed and then surface modified by using a trimethyl silicon chloride compound, or the surface modification of the aerogel powder is dried and oxidized by using an added modifying agent, or the surface modification of the aerogel powder is carried out by using ethanol steam under a high-temperature environment after the aerogel powder is formed, so that the hydrophobic aerogel is formed. However, the surface chemistry of these oxidized aerogels or hydrophobically modified aerogels is not well matched to the spinning plastic. Such aerogel powders therefore cannot be uniformly dispersed in aerogel/plastic composites or aerogel powders with typical post-processing colloids or auxiliaries. Thus, the spinnability of the aerogel composite in the spinning process cannot be satisfied. These phenomena are mainly due to the fact that the aerogel powders have insufficient forces in the matrix, which leads to poor dispersion properties. Leading to difficult subsequent processing of the aerogel powder and poor functional effect of the application.
Disclosure of Invention
Therefore, in order to solve the problems of easy filament breakage of fiber spinning and property degradation of post-processing products caused by uneven dispersion of aerogel powder in the processes of plastic composite processing, textile post-processing and fiber spinning in the past, the present inventors propose a method for preparing functional group modified aerogel particles for producing textiles and fiber spinning by combining a functional group modifier and an aerogel precursor, which comprises the following steps: (1) mixing: mixing a siloxane compound (alkoxy modified siloxane) such as tetramethoxy silane (TMOS) or tetraethoxy silane (TEOS) with a functional group modified siloxane compound (functional group modified siloxane) such as Methyl Trisilicate (MTMS) or propyl amino trisilicate (aminopropyltriethoxy silane (APTE) and adding an organic mixed solvent to form a mixed solution, and adding a functional group modifier in the functional group modified aerogel powder process to modify the functional group of the fine structure in the aerogel system; (2) a hydrolysis step: adding an acid catalyst into the mixed solution to perform hydrolysis reaction, wherein some modified aerogel processes can perform hydrolysis without adding the acid catalyst, and do not need to add the acid catalyst; (3) condensation and dispersion steps: adding an alkali catalyst into the mixed solution to perform condensation reaction, adding a hydrophobic dispersion solvent during the condensation reaction, and stirring at high speed to form dispersed hydrogel particles with the particle size of 10nm-500 mu m during the stirring process of the mixed solution, and then gelling the hydrogel particles to form stable wet hydrogel particles with the particle size of 10nm-500 mu m during the high-speed stirring process. In the condensation and dispersion step, the proportion of the siloxane compound, the functional group modified siloxane compound and the surface functional group modifier in the mixed solution is controlled, the property of the hydrophobic dispersion solvent is regulated so that the functional group of the functional group modified siloxane compound can be presented on the surface of the aerogel molecule, and then the aerogel molecule is promoted to aggregate in the condensation so as to form the functional group modified wet gel particle with the particle diameter of 10nm-500 mu m. (4) Further surface functional group modification step: and adding a surface modifier into the functional group modified wet glue particle dispersion system to further carry out surface modification on the wet glue particles, and adding the surface functional group modifier again in the surface functional group modification step to carry out appearance surface modification on the whole structure of the aerogel so as to ensure that the surface of the micro-pores of the aerogel and the surface of the aerogel main body are fully subjected to surface functional group modification. (5) Solvent evaporation drying step: and then evaporating and drying the solvent under normal pressure, or filtering and drying the filtered wet gel particles to produce uniform modified aerogel powder with specific functional groups for modification and a particle size structure of 10nm-500 mu m. The whole process of the technology is simple and easy, and the aerogel particles with surface functional groups can be prepared. The process speed can be rapidly reduced to 4 to 12 hours, and the surface functional group aerogel particle powder can be prepared, thereby improving the production efficiency.
Further, the group of the functional group-modified silicone compounds can be classified into hydrophilic functional group-modified silicone compounds and hydrophobic functional group-modified silicone compounds, wherein the group of the hydrophilic functional group-modified silicone compounds is a mixture of one or more substances selected from the group consisting of: siloxane compounds (alkoxysilanes) such as Tetramethoxysilane (TMOS) or Tetraethoxysilane (TEOS), hydrophilic functionalized (R-) methyl silicate (R-TMS) or hydrophilic functionalized (R-) ethyl silicate (R-TES), wherein the hydrophilic functional group (R-) substituent group comprises various hydrophilic functional groups such as an acid group-COOH, an amine group-NH 2, an imine group-NH-, a polyamine group-NH 2, a hydroxyl group-OH, an amide group-CONH-, an epoxy group-COH, a urea group-NHCONH-, an isocyanate-N ═ C ═ O, and isocyanuric acid-N-CO-N-, and the number of carbons of the substituent group is from C1 to C8.
Further, the hydrophobic type functional group-modified silicone compound is a mixture of one or more selected from the group consisting of: siloxane compounds (alkoxsilanes) such as Tetramethoxysilane (TMOS) or Tetraethoxysilane (TEOS), hydrophobic functional group modification (R ' -) of methyl silicate (R ' -TMS) or hydrophobic functional group modification (R ' -) of ethyl silicate (R ' -TES), wherein the hydrophobic functional group modification (R ' -) is by a hydrophobic functional group comprising alkyl-CH 3, alkenyl-CH ═ CH2, ester-CO-O-, ether-C-O-C-, aromatic group-C6H 4-, halide group-X, the number of carbons in its hydrophobic group being from C1 to C13; r '-alkenylalkyl silica gels, such as acid-based polydimethyl silica gel (PDMS or DMDMS), or silica gel precursors or R' -alkenylsilane coupling agents.
Further, the organic mixed solvent is one or more selected from the group consisting of: water, alcohols, amines, acids, ketones, ethers, esters, aromatics or alkanes.
Furthermore, the dispersion solvent may comprise a hydrophilic functional group modified siloxane compound dispersion solvent and a hydrophobic functional group modified siloxane compound dispersion solvent according to the process requirements. Adding a large amount of dispersion solvent in the condensation reaction process of the mixture solution of the general siloxane compound and the hydrophilic functional group modified siloxane compound: such as one or more of water, alcohols, ketones, ethers, esters, aromatics and organic halides, the surface layer of the aerogel wet glue particles can have hydrophilic functional group modified groups, such as: and (3) under the action of a dispersion solvent, a hydrophilic functional group modification group is presented on the surface layer of the prepared aerogel wet glue particle shell, and the hydrophilic functional group modification aerogel particle is formed after drying.
Furthermore, a large amount of dispersion solvent is added in the condensation reaction process of the mixture solution of the general siloxane compound and the hydrophobic functional group modified siloxane compound: such as one or more of water, alcohols, ketones, ethers, esters, aromatics, alkanes, halogenated aromatics and halogenated hydrocarbons, the surface layer of the aerogel wet glue particles can have hydrophobic groups, such as: -CH3, -C2H5, -C6H5, CH2X, -C6H4X, the prepared hydrophobic functional group is promoted by the action of a dispersion solvent to enable the hydrophobic functional group modification group to be presented on the surface layer of the shell of the prepared aerogel wet glue particle, and the hydrophobic functional group modification aerogel particle is formed after drying.
Further, subsequent surface functional group modification: and further adding a surface modifier into the mixed functional group modified wet glue particle dispersion system to further modify the functional groups of the wet glue particles, and further modifying the surface functional groups of the structure which is not modified on the surface of the mixed functional group wet glue and is used for modifying the surface of the functional group modified aerogel powder, so that the surface uniform functional groups of the whole structure of the aerogel are modified, and the modifying functions of the fine surface of the aerogel and the surface of the aerogel main body are ensured to be improved.
Furthermore, the solvent evaporation and the drying of the functional group modified aerogel wet glue particles are carried out in a common normal-pressure high-temperature mode in the process. And drying to obtain the functional group modified aerogel powder for the plastic composite or textile fiber. The whole process is simple and can prepare functional group modified aerogel powder with the particle size of 10nm-500 mu m and different surface hydrophilic and hydrophobic properties according to the properties of the base material. The process speed can be rapidly reduced to 3 to 12 hours, and the functional group modified aerogel powder with the functional group with special hydrophilic and hydrophobic properties can be continuously produced and prepared, thereby improving the production efficiency.
The invention has the following effects:
1. according to the preparation method, the siloxane compounds and the functional group modified siloxane compounds in different proportions are mixed in the mixing step, so that the aerogel particles with the fine structure and the special functional groups on the surface can be produced; functional group modified aerogel containing hydrophilic and hydrophobic functional groups is used for obtaining the aerogel particles with excellent plastic compounding and post-processing performance or obviously improved fiber spinning property, and improving the practical property of aerogel powder.
2. The porosity and the size of the holes of the functional group modified aerogel powder particles prepared by the preparation method can be regulated and controlled according to preparation conditions (solvent content, solvent viscosity, acid catalyst, alkali catalyst content, dispersion solvent component, dispersion solvent content, stirring speed and the like).
3. The preparation method of the invention can produce spherical particle-shaped functional group modified aerogel particles with uniform structure and particle size between 10nm-500 mu m by quickly stirring a large amount of dispersion solvents in the condensation dispersion step, the surface layer of the shell of the functional group modified aerogel particles can be hydrophilic functional group or hydrophobic functional group aerogel particles, and the dispersibility of the functional group modified aerogel particles is excellent, so that the aerogel particles with excellent processability or obviously improved fiber spinning property can be obtained, and the practical property of aerogel powder is improved. 4. The surface of the functional group modified aerogel particles of the invention can be modified by hydrophilic functional groups, so that the functional group modified aerogel can be easily and uniformly dispersed in a hydrophilic solvent, such as: water or alcohol, or can be easily combined with hydrophilic base material to disperse, or can be added into base material of plastic, rubber and fibre, etc. which can be combined with hydrophilic functional group to make composite treatment. The aerogel powder plastic base material with excellent dispersion and high content is formed, so that the high porosity inside aerogel in the base material can be kept, and the fiber containing aerogel powder can be directly spun in the subsequent textile post-processing or fiber spinning technology, so that the heat insulation property of the functional group-containing modified aerogel powder in various base materials is improved.
5. The surface of the functional group modified aerogel particles of the present invention can be hydrophobic functional group modified aerogel, so that the functional group modified aerogel can be easily and uniformly dispersed in hydrophobic solvents, such as: hexane or toluene, or can be easily combined with hydrophobic adhesives, plastics, rubber or fiber base materials, and can be uniformly dispersed in base materials such as hydrophobic plastics for compounding. The aerogel powder plastic base material with excellent dispersion and high content is formed, so that the high porosity inside aerogel in the base material can be kept, and the fiber containing aerogel powder can be directly spun in the subsequent textile post-processing or fiber spinning technology, so that the heat insulation property of the functional group-containing modified aerogel powder in various base materials is improved.
6. The invention can shorten the time required by the functional group modification technology by controlling the temperature condition of the functional group modification reaction, and can continuously complete the preparation of the functional group modified aerogel particles within 3 to 8 hours at the fastest speed, thereby improving the production efficiency of the aerogel.
7. The functional group modification of the aerogel powder can be carried out according to the difference of the chemical structures of the added base materials, so that the functional group modified aerogel can be widely applied to plastics: such as polyesters (PET, PBT, PLA …), polyamides (Nylon6, Nylon6, 6, Nylon12 …), polyalkylene hydrocarbons (PE, PP, PEP …), polyacrylic acids (PMMA, PVAC …), etc. The functional group modified aerogel can be widely applied to rubber: such as natural rubber, chlorinated rubber, isoprene rubber, etc. The functional group modified aerogel can be widely applied to lacquer glue: such as poly acrylic glue (PMMA glue), polyurethane glue (PU glue), polyvinyl acetate glue (PVAc glue) and the like.
Drawings
FIG. 1 is a schematic flow chart of the step of modifying hydrophilic functional groups according to the embodiment of the present invention.
FIG. 2 is a schematic flow chart of the step of modifying hydrophobic functional groups according to the embodiment of the present invention.
FIG. 3 is a transmission electron micrograph of the functionally modified aerogel powder prepared according to the present invention.
FIG. 4 is a scanning electron micrograph of a functionally modified aerogel powder prepared according to the present invention.
Fig. 5 is a photograph of hydrophilic amino-functional group modified aerogel powder and amino-functional group modified aerogel powder blended with nylon masterbatch prepared according to the present invention.
Fig. 6 is a photograph of the hydrophobic methyl-functional modified aerogel powder and the polypropylene masterbatch blended with the methyl-functional modified aerogel powder prepared by the present invention.
FIG. 7 is a photograph of the functional modified aerogel powder and spun fiber of the present invention.
FIG. 8 is an electron micrograph of a cut of a functionally modified aerogel powder blended with spun fibers of the present invention.
FIG. 9 is an electron micrograph of a cut surface of a functional group modified aerogel powder blended with spun fibers according to the present invention.
Detailed Description
In combination with the above technical features, the main effects of the functional group modified aerogel particles and the preparation method thereof according to the embodiments of the present invention will be clearly demonstrated in the following embodiments.
Referring first to fig. 1, a method for preparing functional group modified aerogel particles for spinning and fiber spinning according to an embodiment of the present invention is disclosed, which comprises the following steps: a mixing step (S1), a hydrolysis step (S2), a condensation dispersion step (S3), a surface functional group modification step (S4), and a solvent evaporation drying step (S5), wherein:
the mixing step (S1) is: a siloxane compound is mixed with a functional group modified siloxane compound and an organic solvent to form a mixed solution. Examples of the siloxane compound (alkoxysilane) include precursors such as Tetramethylsiloxane (TMOS), Tetraethylsiloxane (TEOS), and methyl orthosilicate. The functional group-modified silicone compound (functional group-modified alkoxysilane); such as hydrophobic functional group-modified silicone compounds: methyl methyltrisilicate (MTMS) or a siloxane compound modified with hydrophilic functional groups such as: such As Propylamine Trisilicate (APTE), and an organic mixed solvent is added to form a mixed solution. The hydrophilic functional group modified siloxane compound is one or more selected from the group consisting of: r-diluted hydrocarbon silicate methyl ester (RTMS) or R-silicate ethyl ester (RTES), R-is a hydrophilic functional group-substituted chain group comprising an acid group-COOH, an amine group-NH 2, an imine group-NH, a hydroxyl group-OH, an amide group-CONH-, an epoxy group-COH, a urea group-NHCONH-, an isocyanate-N ═ C ═ O, isocyanuric acid-N-CO-N-, etc., and the number of carbons in the diluted hydrocarbon chain thereof is from C1 to C8; as in the mixing step (S1). In addition: the hydrophobic functional group modified siloxane compound is one or more selected from the group consisting of: r-dilute hydrocarbyl silicon acid methyl ester (RTMS) OR R-silicon acid ethyl ester (RTES) OR R-dilute hydrocarbyl silica gel OR R-dilute hydrocarbyl silicon coupling agent, R-dilute hydrocarbyl is a functional group-substituted dilute hydrocarbyl chain group comprising alkyl-RCH 3, alkenyl-R-CH 2, ester-R-CO-OR, ether-C-O-C-, aromatic-C6H 4-, halide-X, the number of carbons in the dilute hydrocarbyl chain of which is from C1 to C13; as in the mixing step (S1). The molar content ratio of the siloxane compound to the functional group-modified siloxane compound may be between 0.0 mol% and 100.0 mol%. Adding a functional group modifier to mainly modify the functional group of the fine structure in the aerogel system; the total content of the siloxane compound and the hydrophobic functional group modified siloxane compound mixture is between 1.0 mol% and 60 mol%. The content of the organic mixed solvent is between 99 mol% and 40 mol%.
The hydrolysis step (S2) is: adding an acid catalyst to the mixed solution to perform hydrolysis reaction (hydrolysis). Wherein the ratio of the total content of the siloxane compound and the functional group modified siloxane compound to the content of the acid catalyst is 1: 0.5-1: 0.0001, and the hydrolysis reaction is performed, and some modified aerogel processes can perform hydrolysis without adding the acid catalyst, and do not need to add the acid catalyst.
And the content ratio of the siloxane compound to the acid catalyst is 1: 0.0001 to 1: 0.5. When the ratio of the total content of the siloxane compound and the functional group-modified siloxane compound to the content of the acid catalyst is 1: 0.0001, the hydrolysis reaction time is 360 minutes, and when the ratio of the content of the siloxane compound to the content of the acid catalyst is 1: 0.5, the hydrolysis reaction time is 20 minutes. It is understood that the time required for the hydrolysis reaction decreases as the content of the acid catalyst increases.
The condensation dispersion step (S3) is: adding an alkali catalyst into the mixed solution to perform condensation reaction. The molar ratio of the acid catalyst and ethanol mixed solution to the alkali catalyst water and ethanol mixed solution is, for example, 10: 10 to 10: 40. The molar ratio of the alkali catalyst to the acid catalyst is, for example, 1.0: 1.0 to 3.0: 1.0, and an appropriate amount of alkali catalyst can be added for condensation without adding an acid catalyst hydrolysis process.
In the mixed solution of the alkali catalyst and ethanol, the increase of the content of the alkali catalyst will significantly shorten the condensation reaction time (i.e. the gelation time of the aerogel). (gelation is about 1600 minutes when the ratio of alkali catalyst to acid catalyst is 1.0: 1.0; gelation is reduced to about 5 minutes when the ratio of alkali catalyst to acid catalyst is 3.0: 1.0; condensation is carried out without adding an appropriate amount of alkali catalyst in the hydrolysis process; thus the content of alkali catalyst can be adjusted to adjust the time required for the process; before the condensation reaction in the condensation dispersion step is nearly completed, the mixed solution is formed into sol-like form (sol), the mixed solution is controlled to be sol-like, a large amount of hydrophobic dispersion solvent of incompatible system is added, rapid stirring is carried out at 200rpm to 2000rpm, the mixed solution is influenced by the action force of the dispersion solvent under the rapid stirring condition, so that the sol solution is dispersed into sol-like particles of 10nm to 500 μm, then gelation is carried out to form wet gel particles of pearl or sphere, the particle size of the wet gel particle is about 10nm to 500 μm, the volume ratio (volume ratio) of the mixed solvent to the dispersion solvent is 1.0: 0.5-1.0: 5.0. The higher the content of the dispersion solvent is, the more excellent the uniformity and the dispersibility of the prepared aerogel particles are.
The dispersion solvent for preparing the hydrophilic aerogel particles in the condensation dispersion step (S3) may be water, treated water, deionized water, C1-C16 alcohols, C2-C16 ethers, C3-C16 ketones, C2-C16 esters, C1-C16 acids, C1-C16 amines, or the like. Specifically, for example, water, treated water, deionized water, methanol, ethanol, acetone, butyl ether, ethyl acetate, butyl acetate, formic acid, ammonia water, or a mixture of different components thereof may be used.
The dispersion medium of the hydrophobic aerogel particles in the condensation dispersion step (S3) may be C3-C16 ketones, C2-C16 ethers, C2-C16 esters, C6-C16 aromatics, C5-C16 alkanes, C2-C16 halogenated ethers, C2-C16 halogenated esters, C2-C16 halogenated aromatics, C2-C16 halogenated alkanes, or the like. Specifically, for example, acetone, butyl ether, ethyl acetate, butyl acetate, cyclohexane, n-hexane, toluene, kerosene, and degreasing oil may be used alone or in combination.
The surface functional group modification step (S4) is: the functional group modification of the wet glue particles is further carried out by further adding a surface modifier into the functional group modified wet glue particle dispersion system, and the purpose of the functional group modified aerogel powder is as follows: when the content of the functional group modifier added in the step (1) is more than 50 mol%, further surface modification is not needed; in addition, the purpose of the surface functional group modification step is to perform surface functional group modification of the whole structure of the aerogel so as to ensure that the surface of the micro-pores of the aerogel and the surface of the aerogel main body are fully subjected to functional group modification. The hydrophilic surface functional group modified siloxane compound is one or more selected from the group consisting of: r-diluted hydrocarbon silicate methyl ester (RTMS) or R-silicate ethyl ester (RTES), R-is a hydrophilic functional group-substituted chain group comprising an acid group-COOH, an amine group-NH 2, an imine group-NH, a hydroxyl group-OH, an amide group-CONH-, an epoxy group-COH, a urea group-NHCONH-, an isocyanate-N ═ C ═ O, isocyanuric acid-N-CO-N-, and the like, and the number of carbons in the diluted hydrocarbon chain thereof is from C1 to C8. In addition: the hydrophobic surface functional group modified siloxane compound is one or more selected from the group consisting of: r-dilute hydrocarbyl silicon acid methyl ester (RTMS) OR R-silicon acid ethyl ester (RTES) OR R-dilute hydrocarbyl silica gel OR R-dilute hydrocarbyl silicon coupling agent, R-dilute hydrocarbyl is a functional group-substituted dilute hydrocarbyl chain group comprising alkyl-RCH 3, alkenyl-R-CH 2, ester-R-CO-OR, ether-C-O-C-, aromatic-C6H 4-, halide-X, and the number of carbons in the dilute hydrocarbyl chain thereof is from C1 to C13.
The solvent evaporation drying step (S5) is: after the surface-modified aerogel particles are formed in the dispersion solvent, solvent evaporation can be performed at high temperature to obtain the surface-modified aerogel particles. Or filtering out the surface modified aerogel wet gel particles by a filter, and removing a large amount of dispersion solvent in the surface modified aerogel wet gel system to obtain the surface modified aerogel particles. And further, drying the mixture by using a high-temperature fluidized bed or a constant-temperature drying oven at the drying temperature of 60-250 ℃ to quickly dry the surface modified aerogel particles containing the solvent so as to obtain dry surface modified aerogel powder.
Borrow this, can prepare the porous surface modification aerogel powder granule that sphere shape, size homogeneity are high, can improve the surface modification homogeneity of the outward appearance of surface modification aerogel granule and inner structure on the one hand. In addition, the surface functional group modified aerogel powder can be applied to the mixing of various organic base materials such as plastics, rubber, paint and the like, and the applicability of the aerogel powder is improved. In particular to the preparation of surface functional group modified aerogel powder which can be applied to textile and fiber spinning application, and can obviously improve the addition and mixing uniformity of a large amount of surface functional group modified aerogel powder in plastic post-processing and fiber spinning plastic base materials so as to improve the functionality of the surface functional group modified aerogel powder plastic composite material, or improve the filamentation of aerogel master batches in the spinning process so as to improve the easy mass production of aerogel and obtain the aerogel so as to expand the industrial application scale.
Referring to fig. 2 and fig. 3, a Transmission Electron Microscope (TEM) and a Scanning Electron Microscope (SEM) are used to take the distribution and the appearance size of the surface functional group modified aerogel particles dispersed by stirring at a high speed of 1600rpm, which shows that the appearance structure of the prepared surface functional group modified aerogel particles has a spherical appearance structure with high uniformity and a particle size of about 30-200 nm.
Please refer to fig. 4 and 5, which are photographs of hydrophilic amino surface functional group modified aerogel particles, amino surface functional group modified aerogel mixed Nylon (Nylon6) master batches, hydrophobic methyl surface functional group modified aerogel particles, and methyl surface functional group modified aerogel mixed Polypropylene (PP) master batches. The surface functional group modified aerogel particles prepared by the technology can be highly mixed with different plastic base materials to form plastic master batches of high-concentration aerogel powder.
Referring to fig. 6, it is shown that in the embodiment of the present invention, the surface functional group modified aerogel particles are prepared by using different hydrophilic amino surface functional groups, and the nylon-resistant spinning fiber is prepared by mixing 5%, 10%, and 20% of the amino surface functional group modified aerogel, which shows that the surface functional group modified aerogel spinning fiber can be prepared by using the spinning technology by using the polyester prepared by mixing 5%, 10%, and 20% of the amino surface functional group modified aerogel. The spinning technology of the functional group modified aerogel particles for spinning and fiber spinning can be applied to spinning by a general circular spinning technology, a Special-shaped section spinning technology (Special-shaped section spinning), a core-shell coaxial spinning technology (Two components core-shell coaxial spinning), a Two-component Two-side spinning technology (Two-component Multi-side spinning) or a Multi-component Multi-side spinning technology (Multi-component Multi-side spinning) and the like so as to prepare functional fibers with low density, high heat preservation, high cold resistance, anti-molten drop, high heat insulation and the like.
Referring to fig. 7, 8 and 9, photomicrographs of the cross section of the 20% amino surface functional group modified aerogel hybrid nylon spinning fiber are taken by using a Scanning Electron Microscope (SEM) at different magnifications. Fig. 7 shows a cross section of a 20% amine based surface functional group modified aerogel hybrid nylon spun fiber viewed at 500 times magnification overall. FIG. 8 shows a cross section of a single 20% amino surface functional group modified aerogel hybrid nylon spun fiber viewed at 7,000 times magnification, from which it can be seen that the cross section of the fiber has aerogel particles distributed between it. Fig. 9 shows a photomicrograph of a cross section of the whole amino modified aerogel mixed nylon-spun fiber, which is viewed at a magnification of 50,000 times, wherein the photomicrograph shows that the appearance structure of the amino modified aerogel particles on the cross section of the fiber has high uniformity and a spherical structure with a particle size of about 30-200nm, which is consistent with the appearance structure of the surface functional group modified aerogel powder shown in fig. 2 and 3, and shows that the prepared surface functional group modified aerogel powder is very suitable for fiber spinning.
While the making and using of the present invention and the resulting advantages of the present invention will be apparent from the foregoing description of the preferred embodiments, it will be understood by those skilled in the art that the foregoing descriptions are provided for illustration only and not for the purpose of limiting the invention as defined by the appended claims.
Claims (10)
1. A method for preparing functional group modified aerogel particles for spinning and fiber spinning comprises the following steps:
mixing: mixing a siloxane compound with a functional group modified siloxane compound and an organic solvent to form a mixed solution;
a hydrolysis step: carrying out hydrolysis reaction on the mixed solution;
condensation and dispersion steps: adding an alkali catalyst into the mixed solution to perform condensation reaction, adding a dispersion solvent during the condensation reaction, and rapidly stirring to gelatinize and disperse the mixed solution during stirring to generate functional group modified aerogel particles;
surface modification step: adding a surface modifier into the mixed solution to carry out surface functional group modification on the functional group modified aerogel particles so as to obtain surface modified aerogel wet glue particles;
solvent evaporation drying step: distilling at high temperature or filtering with a filter to obtain the wet gel particles of the surface modified aerogel, and drying at high temperature for solvent drying to obtain a dry powder of the surface modified aerogel.
2. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 1, wherein: the hydrolysis step is to add an acid catalyst into the mixed solution for hydrolysis reaction.
3. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the functional group-modified siloxane compound is a hydrophilic functional group-modified siloxane compound, which is one or more selected from the group consisting of: r-methyl alkenyl silicate or R-ethyl silicate, R-is a hydrophilic functional group substituent group comprising an acid group-COOH, an amine group-NH2imino-NH, hydroxy-OH, amido-CONH-, epoxy-COH, ureido-NHCONH-, isocyanate-N ═ C ═ O, or isocyanuric acid-N-CO-N-, and having a carbon number from C1 to C8.
4. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the functional group-modified siloxane compound is a hydrophobic functional group-modified siloxane compound, which is one or more selected from the group consisting of: r ' -alkenyl methyl silicate, R ' -ethyl silicate, R ' -alkenyl silica gel, or R ' -alkenyl silica coupler, R ' -being a hydrophobic functional group substituent group comprising an alkyl-CH3Alkenyl ═ CH2Ester group-R1-CO-OR 2, ether group-C-O-C-, aromatic-C6H4-, or a halide-X, and has a carbon number of from C1 to C13.
5. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the dispersion solvent is one or more selected from the group consisting of the following hydrophilic solvents: water, treated water, deionized water, alcohols, ethers, ketones, acids, and amines.
6. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the dispersion solvent is one or more selected from the group consisting of the following hydrophobic solvents: ketones, ethers, esters, aromatics, alkanes.
7. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the surface modifier is a hydrophilic surface functional group modifier, which is one or more selected from the group consisting of: r-alkenyl methyl silicate or r-ethyl silicate, r-is a hydrophilic functional group substituent group comprising an acid group-COOH, an amine group-NH2imino-NH, hydroxy-OH, amido-CONH-, epoxy-COH, ureido-NHCONH-, isocyanate-N ═ C ═ O, or isocyanuric acid-N-CO-N-.
8. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the surface modifier is the hydrophobic functional group modified siloxane compound, which is one or more selected from the following substances: r ' -alkenylmethyl silicate, r ' -ethyl silicate, r ' -alkenylsilica gel, or r ' -alkenylsilica coupling agent, r ' -being a hydrophobic functional group substituent comprising an alkyl-CH group3Alkenyl ═ CH2Ester group-R1-CO-OR 2, ether group-C-O-C-, aromatic-C6H4-, or a halide-X.
9. The method for preparing functional group modified aerogel particles for textile and fiber spinning according to claim 2, wherein: the high-temperature drying is carried out at the temperature of 60-250 ℃ and is carried out by utilizing a fluidized bed dryer, a constant-temperature oven, a drum dryer, a stirring dryer, a spray dryer or vacuum drying equipment.
10. The method for preparing functional group modified aerogel particles for spinning and fiber spinning according to any of claims 1 to 8, wherein: and in the condensation reaction process, stirring the mixed solution at a speed of 200rpm to 2000rpm, and gelling the mixed solution in the stirring process to generate functional group modified aerogel particles, wherein the particle size of the functional group modified aerogel particles is 10nm to 500 mu m.
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