CN117165102A - Silicon dioxide dispersoid and preparation method and application thereof - Google Patents
Silicon dioxide dispersoid and preparation method and application thereof Download PDFInfo
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- CN117165102A CN117165102A CN202311112382.2A CN202311112382A CN117165102A CN 117165102 A CN117165102 A CN 117165102A CN 202311112382 A CN202311112382 A CN 202311112382A CN 117165102 A CN117165102 A CN 117165102A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 347
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 121
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229920000728 polyester Polymers 0.000 claims abstract description 78
- 239000003607 modifier Substances 0.000 claims abstract description 60
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 27
- 150000003926 acrylamides Chemical class 0.000 claims abstract description 18
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 15
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 8
- 229920001577 copolymer Polymers 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 9
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- CPLASELWOOUNGW-UHFFFAOYSA-N benzyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CC1=CC=CC=C1 CPLASELWOOUNGW-UHFFFAOYSA-N 0.000 claims description 3
- YGUFXEJWPRRAEK-UHFFFAOYSA-N dodecyl(triethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OCC)(OCC)OCC YGUFXEJWPRRAEK-UHFFFAOYSA-N 0.000 claims description 3
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000006011 modification reaction Methods 0.000 claims description 3
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 3
- FWFUWXVFYKCSQA-UHFFFAOYSA-M sodium;2-methyl-2-(prop-2-enoylamino)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(C)(C)NC(=O)C=C FWFUWXVFYKCSQA-UHFFFAOYSA-M 0.000 claims description 3
- UJQLBTVHLKVNCC-UHFFFAOYSA-M sodium;4-(2-methylprop-2-enoylamino)benzenesulfonate Chemical compound [Na+].CC(=C)C(=O)NC1=CC=C(S([O-])(=O)=O)C=C1 UJQLBTVHLKVNCC-UHFFFAOYSA-M 0.000 claims description 3
- RCYXGFWYLSKLKH-UHFFFAOYSA-M sodium;4-(prop-2-enoylamino)benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(NC(=O)C=C)C=C1 RCYXGFWYLSKLKH-UHFFFAOYSA-M 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000003860 storage Methods 0.000 abstract description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 5
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 description 60
- 239000002245 particle Substances 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 238000005886 esterification reaction Methods 0.000 description 15
- 239000005543 nano-size silicon particle Substances 0.000 description 14
- 238000006068 polycondensation reaction Methods 0.000 description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 12
- 230000032050 esterification Effects 0.000 description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
- 239000012299 nitrogen atmosphere Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 244000025254 Cannabis sativa Species 0.000 description 6
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 6
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 6
- 235000009120 camo Nutrition 0.000 description 6
- 235000005607 chanvre indien Nutrition 0.000 description 6
- 239000011487 hemp Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 239000005457 ice water Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002148 esters Chemical group 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 2
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000008064 anhydrides Chemical group 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical class O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 1
- 241000245240 Lonicera Species 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a silicon dioxide dispersoid and a preparation method and application thereof; the silica dispersion comprises the following components in parts by mass per 100 parts of silica dispersion: 5-20 parts of modified silicon dioxide and 80-95 parts of ethylene glycol; the modified silicon dioxide is prepared by modifying silicon dioxide by a hydrophilic modifier and an oleophylic modifier, wherein the hydrophilic modifier is a copolymer obtained by polymerizing acrylamide derivatives, sodium styrene sulfonate and maleic anhydride, and the oleophylic modifier is an oleophylic silane coupling agent. According to the invention, the hydrophilic modifier and the lipophilic modifier are adopted to sequentially modify the silicon dioxide, so that hydrophilic groups are partially grafted on the surface of the silicon dioxide, and lipophilic groups are partially grafted on the surface of the silicon dioxide; the hydrophilic group can enable the silicon dioxide to be stably dispersed in the glycol, the prepared dispersoid can not generate phenomena of sedimentation, agglomeration, coarsening and the like in the storage or transportation process, and the lipophilic group can enable the silicon dioxide to improve the compatibility of the silicon dioxide and the polymer in the polyester polymerization, so that the silicon dioxide can be uniformly dispersed in the polyester.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a silicon dioxide dispersoid, a preparation method thereof and application thereof in polyester in-situ polymerization.
Background
Synthetic fibers containing more than 85% of polyethylene terephthalate are called polyester fibers in China, and the commodity name is polyester. The polyester is a polymer obtained by polycondensation of polybasic acid and polyhydric alcohol, and the polyester synthesis process has the advantages of a direct esterification method and an ester exchange method, and the direct esterification method has the advantages of low raw material consumption, short reaction time and the like, so that the polyester is a main synthesis process. The main reaction process of the direct esterification method is as follows: firstly, high-purity terephthalic acid and ethylene glycol are subjected to esterification reaction to generate ester and water, and then the generated ester is subjected to polycondensation reaction to obtain polyester and ethylene glycol, wherein the polycondensation comprises pre-polycondensation and final polycondensation. The polyester fiber is a typical hydrophobic fiber, the moisture regain is only about 0.4%, and the polyester fiber has a smooth and non-porous structure, is poor in wearing comfort when being taken as a material for wearing, and is easy to generate stuffiness when being worn in a damp and hot state.
The novel fiber material with high performance, multifunction, light weight and flexibility is an important path for improving the value of the textile industry and meets the upgrading consumption demands of functions, fashion, green and the like. Adding silicon dioxide into polyester fiber, then performing alkali treatment to form micropores on the surface of the fiber, and endowing the fiber with the functions of moisture absorption and quick drying. 3 inventions (publication No. CN104746171A, CN104746172A, CN 104746173A) published by Suzhou Jinhui fiber new material are that nano silicon dioxide is added into China hemp carbon polyester fiber, coffee carbon polyester fiber and hemp stalk carbon polyester fiber, and then alkali washing is carried out to remove the silicon dioxide, so as to obtain the polyester fiber with pores, and the adsorption and moisture absorption capacity of the fiber are improved.
The surface of the silicon dioxide has various hydroxyl groups such as self hydroxyl groups, associated hydroxyl groups, gemini hydroxyl groups and the like, adjacent hydroxyl groups are mutually combined through hydrogen bonds, hydrogen atoms of isolated hydroxyl groups are strong in electropositivity and easy to adsorb with electronegative atoms, the surface hydroxyl groups enable the surface to have chemical adsorption activity, hydrogen bond adsorption is formed when water is encountered, the smaller the particle size is, the larger the specific surface area of the particle is, the higher the surface energy is, the stronger the cohesive force is, the thermodynamic unstable state is achieved, and the particles are easy to agglomerate. After the particle size is reduced by a physical mechanical method, a surfactant is also required to be added or the particles are subjected to surface treatment, so that the phenomena of coarsening and agglomeration or incompatibility with a polymer matrix in the use process are not easy to occur in the subsequent storage. In 3 inventions (publication No. CN104746171A, CN104746172A, CN 104746173A) published by Suzhou Jinhui fiber new material, china hemp carbon/coffee carbon/hemp stalk carbon, a silane coupling agent and nanoscale silicon dioxide powder are directly dispersed, in particular, nanoscale silicon dioxide is attached to the surface pores of the China hemp carbon/coffee carbon/hemp stalk carbon, no pretreatment is carried out on the nanoscale silicon dioxide, and the dispersion of the silicon dioxide in the fiber is uneven.
Chinese patent publication No. CN102330188A discloses a method for preparing nano-silica modified polyester fiber, which comprises adding terephthalic acid and ethylene glycol into a slurry kettle for pulping, then adding nano-silica, nano-zirconium dioxide and titanium dioxide serving as matting agent into the pulping kettle, and esterifying and polycondensing to obtain nano-modified polyester chips. The technology used in this patent is to add nanosilica directly to the polymerizing monomer for polymerization. However, the method of directly adding nano silicon dioxide can not well disperse completely in glycol, is easy to agglomerate in the polymerization and esterification processes, can not well disperse in polyester chips, and can not reflect the effects and characteristics of the nano materials.
The university of east China material physics and chemistry professional Lonicera record, in the graduate paper of research in 2005, industrialized study of Nano silicon dioxide modified PET fiber: the preparation method comprises the steps of proportioning different nano particles, uniformly and stably dispersing the nano particles in glycol through high-speed shearing and stirring, esterifying the glycol with terephthalic acid, performing condensation polymerization to obtain PET/nano silicon dioxide slices in which the nano particles are uniformly dispersed, and performing melt spinning. The method adopts a high-speed shearing method to disperse the nano silicon dioxide into ethylene glycol, however, the method can only disperse the silicon dioxide briefly, but the aggregation, agglomeration and coarsening phenomena of the nano particles can occur after the shearing force is stopped.
The Chinese patent publication No. CN1760443A discloses a preparation method of a polyester nanocomposite material for deeply dyeing fibers, which comprises the steps of adopting nano silicon dioxide as an additive modifier, firstly carrying out organic surface modification on the nano silicon dioxide to uniformly disperse the nano silicon dioxide in glycol which is one of polyester polymerization monomers, adding the prepared nano silicon dioxide/glycol dispersion liquid into a reaction kettle in esterification engineering, polymerizing the mixed nano silicon dioxide/glycol dispersion liquid with another polyester monomer, obtaining the polyester nanocomposite material in the polymerization process, and carrying out high-temperature melt spinning to finally form the polyester nanocomposite fiber; according to the method, nano silicon dioxide particles are added in the polymerization reaction, so that the dye uptake of the dye is greatly improved. Wherein the nano silicon dioxide is subjected to surface organic coating modification, and the organic coating adopts one or more of an organic modifier and a coupling agent to carry out surface modification. However, the use of organic modifiers or coupling agents does not improve the dispersion of nanosilica in ethylene glycol or polyester very well.
The surface of the silicon dioxide particles is generally hydrophilic and has strong polarity, the silicon dioxide particles are easy to combine with moisture in the air, agglomeration is easy to occur, the dispersibility is reduced, and the formed agglomerates are not easy to disperse in organic media with weaker polarity and are not easy to physically adsorb with the organic media. For improving the dispersibility of silica, silane coupling agents, organohalosilanes, silazanes, silicone-based organosilicon compounds, alcohols, organic polymers, and the like are commonly used as modifiers. In the prior art, no report is found on the improvement of the compatibility and the dispersibility of the silicon dioxide and the polyester by using a hydrophilic modifier and an oleophylic modifier to modify the silicon dioxide and using the hydrophilic modifier and the oleophylic modifier in the polyester in-situ polymerization, so that the moisture absorption and quick drying performance of the polyester fiber is improved.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a silicon dioxide dispersoid and a preparation method and application thereof; according to the invention, the hydrophilic modifier and the lipophilic modifier are adopted to sequentially modify the silicon dioxide, so that hydrophilic groups are partially grafted on the surface of the silicon dioxide, and lipophilic groups are partially grafted on the surface of the silicon dioxide; the hydrophilic group can enable the silicon dioxide to be stably dispersed in the glycol, the prepared dispersoid can not generate phenomena of sedimentation, agglomeration, coarsening and the like in the storage or transportation process, and the lipophilic group can enable the silicon dioxide to improve the compatibility of the silicon dioxide and the polymer in the polyester polymerization, so that the silicon dioxide can be uniformly dispersed in the polyester.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a silica dispersion comprises the following components in parts by mass per 100 parts of silica dispersion: 5-20 parts of modified silicon dioxide and 80-95 parts of ethylene glycol; the modified silicon dioxide is prepared by modifying silicon dioxide by a hydrophilic modifier and an oleophylic modifier, wherein the hydrophilic modifier is a copolymer obtained by polymerizing an acrylamide derivative, sodium styrene sulfonate and maleic anhydride, and the oleophylic modifier is an oleophylic silane coupling agent.
Further, the acrylamide derivative has a structure shown in a general formula (I):
in the general formula (I), R 1 、R 2 、R 3 Identical or different and are each independently selected from H or methyl; r is R 4 Is one of alkyl and aromatic hydrocarbon; m is one of Na, K and H. Preferably, the acrylamide derivative is selected from one of 2-acrylamido-2-methylpropanesulfonic acid, sodium 2-acrylamido-2-methylpropanesulfonate, sodium 4-acrylamidobenzenesulfonate and sodium p-methacrylamidobenzenesulfonate.
Preferably, the lipophilic silane coupling agent is at least one selected from phenyl trimethoxy silane, phenyl triethoxy silane, benzyl triethoxy silane, dodecyl trimethoxy silane, dodecyl triethoxy silane, and octadecyl trimethoxy silane.
Further, the silicon dioxide is nano silicon dioxide prepared by a gas phase method, and the particle size is 50-100 nm.
The invention further provides a preparation method of the silica dispersion, which comprises the following steps:
(1) Hydrophilic modification
Taking acrylamide derivatives, sodium styrene sulfonate and maleic anhydride as raw materials, and potassium persulfate and sodium bisulphite as initiators, and heating under the protection of inert gas to perform polymerization reaction to obtain a hydrophilic modifier; adding a silicon dioxide aqueous solution into a hydrophilic modifier, performing hydrophilic modification reaction, and filtering, washing and drying after the reaction to obtain hydrophilic silicon dioxide;
(2) Lipophilicity modification
Adding an oleophylic modifier into a hydrophilic silicon dioxide aqueous solution, heating for reaction under the protection of inert gas, filtering, washing and drying after the reaction to obtain modified silicon dioxide;
(3) Preparation of silica dispersions
Mixing the modified silicon dioxide and ethylene glycol according to the formula amount, and uniformly dispersing by mechanical stirring to obtain the silicon dioxide dispersion.
In the method, the hydrophilic modifier is prepared by polymerizing three monomers under the action of an oxidant through unsaturated double bonds; the anhydride group of the hydrophilic modifier reacts with the hydroxyl group of the silicon dioxide, and the hydrophilic group is grafted to the surface of the silicon dioxide; the methoxy/ethoxy of the lipophilic modifier reacts with the hydroxyl of the silicon dioxide after hydrolysis, and the lipophilic group is grafted to the surface of the silicon dioxide.
In the step (1), the mass ratio of the acrylamide derivative, the sodium styrenesulfonate and the maleic anhydride is (1-3): (1-3): 1.
further, in the method, the mass of the hydrophilic modifier is 1 to 3% of the mass of the silica; the mass of the lipophilic modifier is 1-3% of the mass of the hydrophilic silicon dioxide.
Further, in the step (1), the heating temperature is 50-70 ℃, the polymerization reaction time is 2-6 h, and the hydrophilic modification reaction time is 1-4 h; in the step (2), the heating temperature is 70-90 ℃ and the reaction time is 1-4 h.
The invention further provides application of the silica dispersion in polyester in-situ polymerization, specifically, the silica dispersion is added in the polyester polymerization process, and the adding time can be in the esterification, pre-polycondensation and final polycondensation processes or before the reaction. The silica dispersion of the present invention is obtained by dispersing the modified silica in ethylene glycol which can be used as a raw material for polyester esterification, and therefore the silica dispersion is preferably added before the esterification reaction.
The specific preparation process of the polyester fiber comprises the following steps: raw materials such as silicon dioxide dispersoid, polyethylene glycol, oxidant and the like are subjected to esterification, pre-polycondensation and final polycondensation to obtain polyester melt, and then spinning is carried out to obtain polyester fiber; silica is removed by alkali washing to form micropores on the surface of the polyester fiber.
The beneficial effects of the invention are as follows:
according to the invention, the hydrophilic modifier and the lipophilic modifier are used for sequentially modifying the silicon dioxide, so that hydrophilic groups are partially grafted on the surface of the silicon dioxide, and lipophilic groups are partially grafted on the surface of the silicon dioxide; the hydrophilic group can enable the silicon dioxide to be stably dispersed in the ethylene glycol, and the prepared silicon dioxide dispersion can not generate phenomena of sedimentation, agglomeration, coarsening and the like in the storage or transportation process; the lipophilic group can enable the silica to increase its compatibility with the polymer during the polymerization of the polyester, enabling the silica to be uniformly dispersed in the polyester.
The modified silicon dioxide surface has no hydroxyl groups to crosslink or self-polymerize, the viscosity of the system is reduced, and the sulfonated styrene-maleic anhydride in the hydrophilic modifier can reduce the viscosity of the system, so that the solid content of the silicon dioxide dispersion is improved, and the acrylamide derivative can improve the dispersibility of the silicon dioxide in water and the mechanical property of the polyester fiber.
The silicon dioxide dispersoid disclosed by the invention has the advantages of low viscosity, high solid content, small particle size and good storage stability, is applied to polyester in-situ polymerization, micropores on the fiber surface of the polyester fiber after alkali dissolution are uniformly dispersed, the breaking strength and breaking elongation of the fiber are not obviously changed, the dripping diffusion time is short, the evaporation rate is high, and the moisture absorption quick-drying performance is good.
Drawings
Fig. 1 is an SEM image of microporous polyester fiber No. 1 according to the embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made more apparent and fully by reference to the accompanying drawings, in which it is shown, by way of illustration, only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a silicon dioxide dispersion, which comprises the following components in parts by mass per 100 parts of silicon dioxide dispersion: 5-20 parts of modified silicon dioxide and 80-95 parts of ethylene glycol; the modified silicon dioxide is prepared by modifying silicon dioxide by a hydrophilic modifier and an oleophylic modifier, wherein the hydrophilic modifier is a copolymer obtained by polymerizing an acrylamide derivative, sodium styrene sulfonate and maleic anhydride, and the oleophylic modifier is an oleophylic silane coupling agent.
Wherein the acrylamide derivative has a structure shown in a general formula (I):
in the general formula (I), R 1 、R 2 、R 3 Identical or different and are each independently selected from H or methyl; r is R 4 Is one of alkyl and aromatic hydrocarbon; m is one of Na, K and H.
The acrylamide derivative is preferably one of 2-acrylamido-2-methylpropanesulfonic acid, sodium 2-acrylamido-2-methylpropanesulfonate, sodium 4-acrylamido-benzenesulfonate and sodium p-methacrylamidobenzenesulfonate.
The lipophilic silane coupling agent is preferably at least one of phenyltrimethoxysilane, phenyltriethoxysilane, benzyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, and octadecyltrimethoxysilane.
Wherein the silicon dioxide is nano silicon dioxide prepared by a gas phase method, and the particle size is 50-100 nm.
The invention further provides a preparation method of the silica dispersion, which comprises the following steps:
(1) Hydrophilic modification
The acrylamide derivative, sodium styrenesulfonate and maleic anhydride are mixed according to the mass ratio of (1-3):
(1-3): 1, heating to 50-70 ℃ under the protection of inert gas by taking potassium persulfate and sodium bisulphite as initiators, and carrying out polymerization reaction for 2-6 hours to obtain a hydrophilic modifier; then adding silicon dioxide aqueous solution into the hydrophilic modifier, continuing to react for 1-4 h, and filtering, washing and drying after the reaction to obtain hydrophilic silicon dioxide; the mass of the hydrophilic modifier is 1-3% of the mass of the silicon dioxide;
(2) Lipophilicity modification
Adding an oleophylic modifier into a hydrophilic silicon dioxide aqueous solution, heating to 70-90 ℃ under the protection of inert gas, reacting for 1-4 h, filtering, washing and drying after the reaction to obtain modified silicon dioxide; wherein the mass of the lipophilic modifier is 1-3% of the mass of the hydrophilic silicon dioxide;
(3) Preparation of silica dispersions
Mixing the modified silicon dioxide and ethylene glycol according to the formula amount, and uniformly dispersing by mechanical stirring to obtain the silicon dioxide dispersion.
In the method, the hydrophilic modifier is prepared by polymerizing three monomers under the action of an oxidant through unsaturated double bonds; the anhydride group of the hydrophilic modifier reacts with the hydroxyl group of the silicon dioxide, and the hydrophilic group is grafted to the surface of the silicon dioxide; the methoxy/ethoxy of the lipophilic modifier reacts with the hydroxyl of the silicon dioxide after hydrolysis, and the lipophilic group is grafted to the surface of the silicon dioxide.
The invention further provides application of the silica dispersion in polyester in-situ polymerization, specifically, the silica dispersion is added in the polyester polymerization process, and the adding time can be in the esterification, pre-polycondensation and final polycondensation processes or before the reaction. The silica dispersion of the present invention is obtained by dispersing the modified silica in ethylene glycol which can be used as a raw material for polyester esterification, and therefore the silica dispersion is preferably added before the esterification reaction.
The preparation process of the polyester fiber comprises the following steps: raw materials such as silicon dioxide dispersoid, polyethylene glycol, oxidant and the like are subjected to esterification, pre-polycondensation and final polycondensation to obtain polyester melt, and then spinning is carried out to obtain polyester fiber; silica is removed by alkali washing to form micropores on the surface of the polyester fiber.
The present invention will be described in further detail with reference to the following examples.
Preparation of modified silica
Example 1
0.40g of 2-acrylamide-2-methylpropanesulfonic acid is weighed and dispersed in 5ml of ice water, and the pH value is adjusted to 8.0 by using NaOH solution to obtain solution A; weighing 0.40g of sodium styrene sulfonate and 0.20g of maleic anhydride, dispersing in 10ml of water, adding the solution A, then adding 0.01g of potassium persulfate and 0.01g of sodium bisulfite, heating to 56 ℃ in a nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution containing 50g of silicon dioxide, continuing to react for 2 hours, filtering, washing and drying to obtain hydrophilic silicon dioxide;
1g of phenyl trimethoxysilane was added to a hydrophilic silica aqueous solution containing 50g of hydrophilic silica, heated to 80℃under nitrogen atmosphere, reacted for 2 hours, filtered, washed and dried to obtain modified silica A1.
Example 2
0.20g of 2-acrylamide-2-methylpropanesulfonic acid is weighed and dispersed in 5ml of ice water, and the pH value is adjusted to 8.0 by using NaOH solution to obtain solution A; weighing 0.60g of sodium styrene sulfonate and 0.20g of maleic anhydride, dispersing in 10ml of water, adding the solution A, then adding 0.01g of potassium persulfate and 0.01g of sodium bisulfite, heating to 56 ℃ in a nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution containing 50g of silicon dioxide, continuing to react for 2 hours, filtering, washing and drying to obtain hydrophilic silicon dioxide;
1g of phenyltriethoxysilane is added into a hydrophilic silica aqueous solution containing 50g of hydrophilic silica, and the mixture is heated to 80 ℃ in a nitrogen atmosphere to react for 2 hours, filtered, washed and dried to obtain modified silica A2.
Comparative example 1
0.80g of 2-acrylamide-2-methylpropanesulfonic acid is weighed and dispersed in 10ml of ice water, and the pH value is adjusted to 8.0 by using NaOH solution to obtain solution A; weighing 0.80g of sodium styrene sulfonate, 0.40g of maleic anhydride to disperse in 20ml of water, adding the solution A, then adding 0.02g of potassium persulfate and 0.02g of sodium bisulfite, heating to 56 ℃ in a nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution containing 50g of silicon dioxide, continuing to react for 2 hours, filtering, washing and drying to obtain hydrophilic silicon dioxide.
2g of phenyl trimethoxy silane is added into a hydrophilic silicon dioxide aqueous solution containing 50g of hydrophilic silicon dioxide, the mixture is heated to 80 ℃ in a nitrogen atmosphere, the reaction is carried out for 2 hours, and the modified silicon dioxide B is obtained after filtration, washing and drying.
Comparative example 2
0.40g of 2-acrylamide-2-methylpropanesulfonic acid is weighed and dispersed in 5ml of ice water, and the pH value is adjusted to 8.0 by using NaOH solution to obtain solution A; weighing 0.40g of sodium styrene sulfonate and 0.20g of maleic anhydride, dispersing in 10ml of water, adding the solution A, then adding 0.01g of potassium persulfate and 0.01g of sodium bisulfite, heating to 56 ℃ in a nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution containing 50g of silicon dioxide, continuing to react for 2 hours, filtering, washing and drying to obtain modified silicon dioxide C1.
Comparative example 3
0.80g of 2-acrylamide-2-methylpropanesulfonic acid is weighed and dispersed in 10ml of ice water, and the pH value is adjusted to 8.0 by using NaOH solution to obtain solution A; weighing 0.80g of sodium styrene sulfonate, 0.40g of maleic anhydride to be dispersed in 20ml of water, adding the solution A, adding 0.02g of potassium persulfate and 0.02g of sodium bisulfite, heating to 56 ℃ in a nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution with the silicon dioxide mass of 50g, continuing to react for 2 hours, filtering, washing and drying to obtain modified silicon dioxide C2.
Comparative example 4
1g of phenyl trimethoxysilane is added into a silicon dioxide aqueous solution with the mass of 50g of silicon dioxide, the mixture is heated to 80 ℃ in a nitrogen atmosphere, the reaction is carried out for 2 hours, and the modified silicon dioxide D1 is obtained after filtration, washing and drying.
Comparative example 5
2g of phenyl trimethoxy silane is added into a silicon dioxide aqueous solution with the mass of 50g of silicon dioxide, the mixture is heated to 80 ℃ in a nitrogen atmosphere, the reaction is carried out for 2 hours, and the modified silicon dioxide D2 is obtained after filtration, washing and drying.
Comparative example 6
Weighing 0.40g of sodium styrene sulfonate, 0.20g of maleic anhydride to be dispersed in 10ml of water, adding 0.01g of potassium persulfate and 0.01g of sodium bisulfite, heating to 56 ℃ in nitrogen atmosphere, and carrying out polymerization reaction for 4 hours to obtain a hydrophilic modifier; then adding a silicon dioxide aqueous solution with the silicon dioxide mass of 50g, continuing to react for 2 hours, filtering, washing and drying to obtain hydrophilic silicon dioxide;
1g of phenyl trimethoxysilane was added to a hydrophilic silica aqueous solution containing 50g of hydrophilic silica, heated to 80℃under nitrogen atmosphere, reacted for 2 hours, filtered, washed and dried to obtain modified silica D3.
Preparation and testing of silica dispersions
The modified silica prepared in examples 1 to 2 and comparative examples 1 to 6, and the untreated silica (E) purchased directly were uniformly dispersed with ethylene glycol in the mass ratio shown in Table 1 by mechanical stirring to obtain silica dispersions having numbers 1 to 11.
TABLE 1 silica Dispersion component mass ratio
Viscosity and particle size tests were performed on the prepared silica dispersions No. 1-10, and viscosity and particle size were tested after 30 days of storage, and the test data are shown in Table 2; since the slurry obtained from the silica dispersion No. 11 was pasty, and poor in fluidity, no relevant test was conducted.
TABLE 2 results of silica Dispersion Performance test
As is clear from Table 2, the silica dispersions No. 1 to No. 5 have low dispersion viscosity and small particle size in ethylene glycol due to the hydrophilic groups grafted on the silica surface; after 30 days of storage, the viscosity and particle size did not change much. The silicon dioxide dispersion of 6 to 7 has larger dispersion viscosity and larger particle diameter in glycol because the surface of the silicon dioxide is grafted with lipophilic groups; after 30 days of large storage, the viscosity and particle size change greatly. Since the hydrophilic modifier is not added with the acrylamide derivative, the viscosity and the particle size of the silica in ethylene glycol are larger than those of the silica dispersion No. 1, and the viscosity and the particle size change greatly after 30 days of storage. Silica of silica dispersion No. 9 is a commercial product, and the viscosity and particle size of silica are large due to self-crosslinking; after 30 days of storage, the viscosity and particle size varied greatly. Compared with the silica dispersion No. 1, the silica dispersion No. 10 has the advantages that the content of silica is increased, the viscosity is slightly increased, and the particle size is slightly changed; after 30 days of storage, the viscosity and particle size did not change much. The silica of silica dispersion No. 11 is commercially available, and the resulting slurry was in the form of a paste, poor in fluidity, and not subjected to the relevant test.
Preparation and performance test of microporous polyester fiber
The silica dispersion with the serial number of 1-10 is added into a polyester reaction vessel (wherein the mass of silica in the silica dispersion accounts for 1 percent of the total mass of terephthalic acid and ethylene glycol, the mol ratio of terephthalic acid to ethylene glycol is 1:1.2, and the mass of catalyst tetrabutyl titanate accounts for 0.2 percent of the mass of terephthalic acid), and polyester melt is obtained through esterification (the reaction temperature is 265 ℃, the reaction pressure is 150 kPa), precondensation (the reaction temperature is 260 ℃, the reaction pressure is 3 kPa) and final polycondensation (the reaction temperature is 265 ℃ and the reaction pressure is 100 Pa). Spinning at 255 deg.c and winding speed of 4500m/min to obtain polyester fiber. And (3) alkaline washing the polyester fiber in a sodium hydroxide solution with the concentration of 1mol/L at the temperature of 100 ℃ for 120min, and then washing and drying the polyester fiber to obtain the microporous polyester fiber with the serial number of 1-10. Microporous polyester fibers having a number of 1 to 10, and conventional polyester fibers having a number of 11 (no silica dispersion added in polymerization) were tested as follows:
breaking strength and elongation at break: reference is made to GB/T14344-2022 chemical fibre filament tensile property test method;
drip diffusion time and evaporation rate: evaluation of moisture absorption and quick drying Properties of textiles with reference to GB/T21655.1-2008 part 1: single item combination test method.
The test results are shown in Table 3.
TABLE 3 polyester fiber Performance test results
| Polyester fiber serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 |
| Breaking strength (cN/dtex) | 3.9 | 4.0 | 2.4 | 2.5 | 2.4 | 2.3 | 2.1 | 2.2 | 2.6 | 3.8 | 4.2 |
| Elongation at break (%) | 35 | 36 | 23 | 25 | 24 | 23 | 21 | 21 | 27 | 34 | 39 |
| Drip diffusion time(s) | 0.3 | 0.3 | 4.5 | 4.6 | 4.8 | 5.1 | 5.2 | 4.7 | 4.2 | 0.3 | 6.6 |
| Evaporation rate (g/h) | 1.06 | 1.06 | 0.16 | 0.17 | 0.15 | 0.15 | 0.14 | 0.15 | 0.21 | 1.05 | 0.11 |
The modified silicon dioxide A1 or A2 is added in the polymerization of the polyester fibers No. 1, no. 2 and No. 10, the content of the modified silicon dioxide A1 or A2 in the polyester fibers is the same, and the breaking strength, the breaking productivity, the drip diffusion time and the evaporation rate of the two fibers are basically the same.
Compared with the No. 11 polyester fiber, the breaking strength and the breaking productivity of the No. 1, no. 2 and No. 10 fibers are basically the same, the dripping diffusion time is short, the evaporation rate is high, and the silica dispersion prepared by the invention is applied to the polyester fiber, so that the moisture absorption and perspiration performance of the fiber is improved, and the mechanical property of the fiber is not greatly influenced.
Compared with the No. 1 polyester fiber, the No. 3-5 polyester fiber has poor breaking strength, breaking productivity, drip diffusion time and evaporation rate, and the poor mechanical properties and moisture absorption and sweat release properties of the fiber are caused by poor dispersion performance of the silica in the No. 3-5 silica dispersion in polyester synthesis.
Compared with the No. 1 polyester fiber, the No. 6-7 polyester fiber has poor breaking strength, breaking productivity, drip diffusion time and evaporation rate, and the poor mechanical properties and moisture absorption and perspiration properties of the fiber are caused by poor dispersion performance of the No. 6-7 silicon dioxide dispersion and poor dispersion in polyester polymerization.
The polyester fiber No. 8 is inferior in breaking strength, breaking productivity, drip diffusion time, evaporation rate as compared with the polyester fiber No. 1, because the modifier of the silica dispersion No. 8 does not contain an acrylamide derivative, and the silica dispersion is relatively poor.
Compared with the No. 1 polyester fiber, the commercial silicon dioxide used by the No. 9 polyester fiber has poor dispersion performance in glycol and polyester, and the No. 9 polyester fiber has poor breaking strength, breaking productivity, drip diffusion time and evaporation rate.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all modifications or equivalent arrangements using the teachings of this invention, or direct or indirect application in other related arts, are included within the scope of this invention.
Claims (10)
1. A silica dispersion characterized by comprising the following components in parts by mass per 100 parts of silica dispersion: 5-20 parts of modified silicon dioxide and 80-95 parts of ethylene glycol; the modified silicon dioxide is prepared by modifying silicon dioxide by a hydrophilic modifier and an oleophylic modifier, wherein the hydrophilic modifier is a copolymer obtained by polymerizing an acrylamide derivative, sodium styrene sulfonate and maleic anhydride, and the oleophylic modifier is an oleophylic silane coupling agent.
2. The silica dispersion according to claim 1, wherein the acrylamide derivative has a structure represented by the general formula (i):
in the general formula (I), R 1 、R 2 、R 3 Identical or different and are each independently selected from H or methyl; r is R 4 Is one of alkyl and aromatic hydrocarbon; m is one of Na, K and H.
3. The silica dispersion according to claim 1, wherein the acrylamide derivative is selected from one of sodium 2-acrylamido-2-methylpropanesulfonate, sodium 4-acrylamido-benzenesulfonate, sodium p-methacrylamidobenzenesulfonate.
4. The silica dispersion according to claim 1, wherein the lipophilic silane coupling agent is selected from at least one of phenyltrimethoxysilane, phenyltriethoxysilane, benzyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, octadecyltrimethoxysilane.
5. The silica dispersion of claim 1 wherein the silica is nanosilica prepared by a gas phase process.
6. A process for the preparation of a silica dispersion according to any one of claims 1 to 5, comprising the steps of:
(1) Hydrophilic modification
Taking acrylamide derivatives, sodium styrene sulfonate and maleic anhydride as raw materials, and potassium persulfate and sodium bisulphite as initiators, and heating under the protection of inert gas to perform polymerization reaction to obtain a hydrophilic modifier; adding a silicon dioxide aqueous solution into a hydrophilic modifier, performing hydrophilic modification reaction, and filtering, washing and drying after the reaction to obtain hydrophilic silicon dioxide;
(2) Lipophilicity modification
Adding an oleophylic modifier into a hydrophilic silicon dioxide aqueous solution, heating for reaction under the protection of inert gas, filtering, washing and drying after the reaction to obtain modified silicon dioxide;
(3) Preparation of silica dispersions
Mixing the modified silicon dioxide and ethylene glycol according to the formula amount, and uniformly dispersing by mechanical stirring to obtain the silicon dioxide dispersion.
7. The method of producing a silica dispersion according to claim 6, wherein in the step (1), the mass ratio of the acrylamide derivative, sodium styrenesulfonate, and maleic anhydride is (1 to 3): (1-3): 1.
8. the method for producing a silica dispersion according to claim 6, wherein the mass of the hydrophilic modifier is 1 to 3% of the mass of silica; the mass of the lipophilic modifier is 1-3% of the mass of the hydrophilic silicon dioxide.
9. The method for producing a silica dispersion according to claim 6, wherein in the step (1), the heating temperature is 50 to 70 ℃, the polymerization time is 2 to 6 hours, and the hydrophilic modification time is 1 to 4 hours; in the step (2), the heating temperature is 70-90 ℃ and the reaction time is 1-4 h.
10. Use of the silica dispersion according to any one of claims 1 to 5 in polyester in situ polymerization.
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| CN119059764B (en) * | 2024-11-04 | 2025-03-14 | 克拉玛依市红都有限责任公司 | Plugging agent for carbon dioxide gas flooding well and preparation method thereof |
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