CN116004036A - Preparation method of sol-gel method film opening agent - Google Patents
Preparation method of sol-gel method film opening agent Download PDFInfo
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- CN116004036A CN116004036A CN202211488469.5A CN202211488469A CN116004036A CN 116004036 A CN116004036 A CN 116004036A CN 202211488469 A CN202211488469 A CN 202211488469A CN 116004036 A CN116004036 A CN 116004036A
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- Prior art keywords
- sol
- sulfuric acid
- opening agent
- water glass
- silica
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000003980 solgel method Methods 0.000 title abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 155
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 116
- 238000005406 washing Methods 0.000 claims abstract description 54
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000741 silica gel Substances 0.000 claims abstract description 32
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 32
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 29
- 230000032683 aging Effects 0.000 claims abstract description 25
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 11
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 8
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000012986 modification Methods 0.000 claims abstract description 4
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 58
- 239000000243 solution Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 230000001804 emulsifying effect Effects 0.000 claims description 18
- 239000000499 gel Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 14
- 239000001099 ammonium carbonate Substances 0.000 claims description 14
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 12
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 12
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 10
- 150000003863 ammonium salts Chemical class 0.000 claims description 10
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 5
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 2
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 claims description 2
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 239000000126 substance Substances 0.000 abstract description 31
- 239000002985 plastic film Substances 0.000 abstract description 10
- 229920006255 plastic film Polymers 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000011668 ascorbic acid Substances 0.000 abstract description 4
- 235000010724 Wisteria floribunda Nutrition 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 42
- 235000012239 silicon dioxide Nutrition 0.000 description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 14
- 238000003756 stirring Methods 0.000 description 12
- 239000012498 ultrapure water Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- 239000004033 plastic Substances 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 8
- 238000010902 jet-milling Methods 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 238000001694 spray drying Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000007822 coupling agent Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004964 aerogel Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of polymer material processing, and particularly relates to a preparation method of a sol-gel method film opening agent, which comprises the following steps of; s1, forming silica sol by pressurizing and convection of a water glass solution and sulfuric acid; s2, heating the silica sol obtained in the step S1, adjusting the pH to be alkaline, then adding the silane coupling agents A and B for modification, adjusting the pH to be acidic after aging is completed, and aging to form silica gel; s3, washing the silica gel obtained in the step S2, and uniformly dispersing the washed silica gel; s4, drying the slurry after the dispersion in the step S3, and crushing to obtain the final product. The physical and chemical indexes of the opening agent prepared by the technical scheme of the invention are close to those of Fuji SY340 and Graves E300, and the film opening agent has uniform particles and easy dispersion, and has good transparency and processability in the production of polyethylene terephthalate plastic films.
Description
Technical Field
The invention belongs to the technical field of polymer material processing, and particularly relates to a preparation method of a sol-gel method film opening agent.
Background
In the production and storage processes of plastics, adhesion is easy to occur between film layers under hot pressing or object pressing, the adhesion between films is light, so that the unreeling speed of plastics is influenced, for example, the unreeling speed of plastics is influenced when the adhesion between films is light in the processes of rolling, slitting, packaging and the like, and the plastics can not be unfolded for use when the adhesion between films is heavy. The film adhesion is mainly caused by the fact that a vacuum closed state is formed between films after the films are closed, the films are not easy to separate, a large number of exposed molecular chains are arranged on the surfaces of the films after the films are formed, and the macromolecular chains are mutually wound and adhered after the films are closed, so that the films cannot be opened, the plastic films are mutually adhered to bring difficulty to automatic packaging application, and an opening agent is added in the plastic production process to solve the problem, so that the openness of the films is improved.
The earliest used opening agents are inorganic talcum powder, diatomite and the like, the diatomite and the talcum powder mainly have low pore volume and poor opening property, and the produced film has poor transparency, which are abandoned by people, and the early stages of the opening agents are developed into organic oleic acid phtalamine, erucic acid phtalamine EBS derivatives and the like. The organic opening agent has the defects that a large amount of precipitate exists on the surface of the film, the printability, the heat sealability and the color of the film are affected, the use of the film is further affected, the silicon dioxide has high chemical purity, no toxicity, no harm and no pollution, the refractive index of the organic opening agent is close to that of the plastic materials such as PE, PP, PET, PA, the influence on the optical performance is small, and the high-quality opening agent which is relatively wide in the plastic industry of the opening agent is widely used in the field of various plastic films at present.
Chinese patent CN109705402A discloses a preparation method of aerogel film opening agent, which comprises the steps of adding sulfuric acid to form gel, beating glue, raising the temperature to 70-90 ℃, simultaneously adding sulfuric acid and water glass solution to keep the pH value to 8-10, adjusting the temperature to 85-95 ℃ after parallel flow is completed, adding silane coupling agent, aging for 2-4 hours, adjusting the pH value to 2-4, aging, washing with 1-3% dilute sulfuric acid, washing filter cakes according to ammonium salt solution, washing with water, finally dispersing with a dispersing machine and an emulsifying machine together, spraying and crushing to obtain the particle size of 3.3-3.5 um, wherein the product is successfully used in polypropylene plastic film systems at present, but has the disadvantages of feedback bulk density bias, physical and chemical indexes with Graves E300 and application performances in polyethylene terephthalate plastic films. Chinese patent CN110229380a discloses a preparation method of high-efficiency high-transparency silica plastic film opening agent, which adopts the scheme that the temperature of the bottom water is raised, and ammonium bicarbonate and water glass solution are added to obtain a first reaction solution; the pH value of the reaction and flowing to the second reaction liquid is: 3.0 to 5.0, and then aging for 30 minutes to obtain reaction slurry; the reaction slurry is washed by adding water, and the high-efficiency and high-transparency silica plastic film opening agent is prepared by pulping, atomizing, drying and crushing.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a sol-gel method film opening agent, and the film opening agent prepared by the method has uniform particles, is easy to disperse, and has good transparency and processability in the production of polyethylene terephthalate plastic films.
The primary aim of the invention is to provide a preparation method of a sol-gel method film opening agent.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a sol-gel method film opening agent comprises the following steps:
s1, forming silica sol by pressurizing and convection of a water glass solution and sulfuric acid;
s2, heating the silica sol obtained in the step S1, adjusting the pH to be alkaline, then adding a silane coupling agent A and a silane coupling agent B to carry out surface modification on the silica, adjusting the pH to be acidic after aging is completed, and aging to form silica gel;
s3, washing the silica gel obtained in the step S2, and uniformly dispersing the washed silica gel;
s4, drying the slurry after the dispersion in the step S3, and crushing to obtain the slurry;
in the step S2, the silane coupling agent a is one of KH520 (γ -aminopropyl methyl diethoxysilane), KH530 (γ -aminopropyl methyl dimethoxysilane), KH540 (γ -aminopropyl trimethoxysilane), KH550 (γ -aminopropyl triethoxysilane), KH560 (γ -glycidoxypropyl), KH570 (γ - (methacryloyloxy) propyl trimethoxysilane), and the silane coupling agent B is one of KH580 (3-mercaptopropyl trimethoxysilane) and KH590 (3-mercaptopropyl triethoxysilane).
The pressurizing convection mode of the invention is that when the prepared water glass and sulfuric acid solution are injected into the reaction vessel at the same time, a pressurizing pump is arranged in the water glass and sulfuric acid flow pipeline to increase the flow velocity, and the pressurizing convection accelerates the rapid formation of the primary particles of the silicon dioxide, thereby the rapid formation of the network structure of the silicon dioxide, the richness of the network structure of the silicon dioxide is increased along with the rapid formation of the network structure of the silicon dioxide, and the porosity of the silicon dioxide is increased.
Preferably, the silica modulus of the water glass solution in the step S1 is 3.20-3.40, the concentration is 10-20 wt%, and the sulfuric acid concentration is 30-50 wt%.
Preferably, the content of Fe element in the water glass solution in the step S1 is less than or equal to 15ppm, the content of Al element is less than or equal to 1ppm, the content of Ca element is less than or equal to 1ppm, the content of Mg element is less than or equal to 1ppm, and the solubility of solid water glass is more than or equal to 99.5%.
Preferably, the flow pipeline pressure of the water glass and the sulfuric acid after the pressurization in the step S1 is kept between 0.5Mpa and 1Mpa, the flow rate of the water glass solution is between 180L/h and 230L/h, and the flow rate of the sulfuric acid is between 30L/h and 50L/h.
Preferably, the total addition amount of the silane coupling agent in the step S2 is 0.50-0.80 wt% of the dry basis, wherein the addition mass ratio of the silane coupling agent A to the silane coupling agent B is 4:1.
Preferably, in the step S2, the pH is adjusted to be alkaline to a value of 8-10, and the pH is adjusted to be acidic to a value of 2-4.
Preferably, the washing in the step S3 is to use pure water, sulfuric acid solution, ammonium salt aqueous solution and pure water respectively at a time interval of 1:5:3:1 in the washing sequence until the conductivity of the silica gel is below 50 us/cm.
More preferably, the conductivity of the pure water is lower than 5us/cm, the temperature is 50-80 ℃, the concentration of the sulfuric acid solution is 30-60% of the solution, the ammonium salt is one of ammonium sulfate, ammonium bisulfate, ammonium carbonate and ammonium bicarbonate, and the weight ratio of the ammonium salt to water in the ammonium salt water solution is 0.05-0.10: 1.
preferably, in the dispersing in the step S3, under the combined action of the dispersing machine and the emulsifying machine, the rotation degree of the dispersing machine is 1500-2500 rpm, the rotation degree of the emulsifying machine is 3000-5000 rpm, and the combined action time is 30-60 minutes, more preferably 45 minutes.
Under the combined action of the dispersing machine and the emulsifying machine, the filter cake is uniform and fine in aerogel particles, so that the aerogel film opening agent has good dispersibility and filterability.
The invention also aims to provide the film opening agent prepared by the method.
The invention also provides application of the film opening agent in preparation of polyethylene terephthalate film to improve film performance.
Compared with the prior art, the invention has the beneficial effects that:
(1) The high-purity water glass is used as a raw material for preparing the silicon dioxide by a sol-gel method, wherein the content of Fe element of the high-purity water glass is less than or equal to 15ppm, the content of Al element is less than or equal to 1ppm, the content of Ca element is less than or equal to 1ppm, the content of Mg element is less than or equal to 1ppm, the solubility of solid water glass is more than or equal to 99.5%, the content of iron and other miscellaneous elements is smaller, and the fixed water glass has higher solubility, so that the appearance of the synthesized opening agent master batch is whiter, lighter in color and higher in transparency can be ensured.
(2) The method adopts the high-pressure convection mode of high-purity water glass and sulfuric acid to react, can ensure that the generated silica gel has uniform structure and high stability, and is easy to disperse in the process of synthesizing the opening agent.
(3) The application adopts pure water washing to reduce sulfate ions of silicon dioxide, ammonium salt solution washing in which ammonium ions and sodium ions are mutually exchanged to increase the washing speed, saves the washing dosage, can also ream silicon dioxide particles to a certain extent, and sulfuric acid solution washing can reduce iron elements in sulfuric acid and water glass and iron elements and other hetero-elements in the production process to a certain extent, thereby ensuring the appearance and color of the opening agent master batch.
(4) The silica gel is treated simultaneously by the silane coupling agent A and the silane coupling agent B, wherein the silane coupling agent A can improve the affinity degree of silica particles and an organic polymer, improve the antistatic property, the lubricating property and the moisture-proof property of the silica particles, reduce the friction coefficient and the bonding resistance, and the silane coupling agent B can improve the hardness of a silica structure, so that the silica is better dispersed in an opening agent system, and the silica and the organic polymer cooperate to achieve better opening and dispersing effects.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in conjunction with examples of the present invention and comparative examples, and it is apparent that the described examples are only some of the examples of the present invention, but not all of the examples. 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 test methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
Example 1
At 30 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 1Mpa, high-purity water glass 16L with the flow rate of 200L/h, the silicon dioxide concentration of 15wt percent and the modulus of 3.25 and sulfuric acid solution with the flow rate of 50L/h and the concentration of 30wt percent are simultaneously injected into a 50L stirring reaction vessel, 4L of sulfuric acid solution with the flow rate of 50L/h and the concentration of 30wt percent are added for 6min to form silica sol, caustic soda is added to adjust the pH value to 9.0 after the silica sol is formed, the temperature is increased to 95 ℃, KH540 (gamma-aminopropyl trimethoxysilane) with the silicon dioxide content of 0.40wt percent and KH580 (3-mercaptopropyl trimethoxysilane) with the silicon dioxide content of 0.10wt percent are added, stirring and ageing are carried out for 3h under the condition, sulfuric acid is added to adjust the pH value to 3 after ageing is finished, ageing is carried out for 1 h, the silica gel is formed, after the gel is cooled to 60 ℃, water washing is carried out by pumping into a filter pressing plate frame, and according to pure water and 50% sulfuric acid solution with the temperature of 60 ℃ and ammonium bicarbonate: water was 0.05:1, washing the silica gel by pure water at the temperature of 60 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 5 hours, the washing time is lower than 50us/cm, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine at the same time, the rotating speed of the dispersing machine is 2500 r/min, and the speed of the emulsifying machine is 3000 r/min. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product are tested by the method and standard:
(1) Porosity test: full-automatic specific surface area and porosity analyzer microphone: triStar II 3020;
(2) Average particle diameter: laser particle size analyzer: markov 3000;
(3) Oil absorption value: picking knife method: 1g of silica absorbs dibutyl phthalate; reference is made to the row label HG/T3072-2008;
(4) Iron content testing: o-phenanthroline spectrophotometry;
(5) Conductivity test: lei Ci DDS-11A;
(6) Bulk density testing: bulk density refers to the density obtained by dividing the powder mass by the volume V of the container occupied by the powder, also known as bulk density;
the physicochemical properties of the seven parallel products are shown in Table 1.
TABLE 1
Example 2
At 40 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 0.5Mpa, high-purity water glass 18L with the flow rate of 230L/h, the silicon dioxide concentration of 10wt percent and the modulus of 3.25 and sulfuric acid solution with the flow rate of 50L/h and the concentration of 30wt percent are simultaneously injected into a 50L stirring reaction vessel, 5L of sulfuric acid solution with the flow rate of 50L/h and the concentration of 30wt percent are added for 5min to form silica sol, caustic soda is added to adjust the pH value to 10.0 after the silica sol is formed, the temperature is increased to 80 ℃, KH550 (gamma-glycidoxypropyl) with the silicon dioxide content of 0.64wt percent and KH580 (3-mercaptotrimethoxysilane) with the silicon dioxide content of 0.16wt percent are added, stirring and ageing are carried out for 2h under the conditions, sulfuric acid is added to adjust the pH value to 4 after the ageing is finished, ageing is carried out for 0.5 h, the silica gel is formed, the temperature is cooled to 70 ℃, and the silica sol is pumped into a filter pressing plate frame for water washing, and the pure water solution with 50 percent of sulfuric acid and ammonium bicarbonate are carried out according to 60 ℃ to the temperature: water was 0.05:1, washing the silica gel by pure water at the temperature of 60 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 5 hours, the washing time is lower than 50us/cm, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine at the same time, the rotating speed of the dispersing machine is 2500 r/min, and the speed of the emulsifying machine is 5000 r/min. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product are shown in Table 2, and the physical and chemical properties of seven parallel products are the same as those of example 1.
TABLE 2
Example 3
At 20 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 1Mpa, high-purity water glass 14L with the flow rate of 180L/h, the silicon dioxide concentration of 20wt percent and the modulus of 3.25 and sulfuric acid solution with the flow rate of 30L/h and the concentration of 30wt percent are simultaneously injected into a 50L stirring reaction vessel, 3L of sulfuric acid solution with the flow rate of 30wt percent and the temperature of 3L of sulfuric acid solution is increased to 95 ℃ for 8min to form silica sol, caustic soda is added to adjust the pH value to 8.0 after the silica sol is formed, KH560 (gamma-aminopropyl triethoxysilane) with the silicon dioxide content of 0.56wt percent and KH590 (3-mercaptopropyl triethoxysilane) with the silicon dioxide content of 0.14wt percent are added, stirring and ageing are carried out for 5h under the conditions, sulfuric acid is added to adjust the pH value to 2 after the ageing is finished, ageing is carried out for 1.5 h, silica gel is formed, after the gel is cooled to 50 ℃, and the plate frame is pumped for water washing, and pure water solution with the temperature of 80 ℃ and ammonium bicarbonate is added: water was 0.10:1, washing the silica gel by pure water at 80 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 3 hours, the washing time is lower than 50us/cm of conductivity, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine at the same time, the rotating speed of the dispersing machine is 1500 revolutions per minute, and the speed of the emulsifying machine is 5000 revolutions per minute. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 3.
TABLE 3 Table 3
Example 4
At 25 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 0.9Mpa, high-purity water glass 16L with the flow rate of 200L/h, the silicon dioxide concentration of 15wt percent and the modulus of 3.20 and sulfuric acid solution with the flow rate of 40L/h and the concentration of 40wt percent are simultaneously injected into a 50L stirring reaction vessel, 4L of sulfuric acid solution with the flow rate of 40L/h and the concentration of 40wt percent are added for 5min to form silica sol, caustic soda is added to adjust the pH value to 9.5 after the silica sol is formed, the temperature is increased to 90 ℃, KH530 (gamma- (methacryloyloxy) propyl trimethoxysilane) with the silicon dioxide content of 0.48wt percent and KH590 (3-mercaptopropyl triethoxysilane) with the silicon dioxide content of 0.12wt percent are added, stirring and ageing are carried out under the conditions, sulfuric acid is added to adjust the pH value to 4 after ageing is finished, the silica gel is formed, the temperature is cooled to 70 ℃ after the gel is finished, the silica sol is pumped into a filter pressing plate frame for water washing, pure water, 60% sulfuric acid solution and ammonium bicarbonate are added according to 70 ℃ to the pure water and 60% sulfuric acid solution: water was 0.08:1, washing the silica gel by pure water at 70 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 4 hours, the washing time is lower than 50us/cm of conductivity, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine at the same time, the rotating speed of the dispersing machine is 2000 revolutions per minute, and the speed of the emulsifying machine is 3000 revolutions per minute. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 4.
TABLE 4 Table 4
Example 5
At 29 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 0.7Mpa, high-purity water glass 15L with the flow rate of 190L/h, the silicon dioxide concentration of 18wt percent and the modulus of 3.30 and sulfuric acid solution with the flow rate of 45L/h and the concentration of 40wt percent are simultaneously injected into a 50L stirring reaction vessel, 3.8L of sulfuric acid solution with the flow rate of 40wt percent are added for 6min to form silica sol, caustic soda is added to adjust the pH value to 9.5 after the silica sol is formed, the temperature is raised to 95 ℃, KH570 (gamma- (methacryloyloxy) propyl trimethoxysilane) with the silicon dioxide content of 0.64wt percent and KH580 (3-mercaptopropyl trimethoxysilane) with the silicon dioxide content of 0.16wt percent are added, stirring and aging are carried out for 5h under the condition, sulfuric acid is added to adjust the pH value to 3 after aging is completed, filter pressing gel is formed, the temperature is cooled to 60 ℃ after the gel is completed, water washing is carried out by pumping into a plate frame, and pure water and ammonium bicarbonate solution with the temperature of 30 percent is carried out according to 50 ℃: water was 0.05:1, washing the silica gel by pure water at 50 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 5 hours, the washing time is lower than 50us/cm, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine at the same time, the rotating speed of the dispersing machine is 2000 revolutions per minute, and the speed of the emulsifying machine is 5000 revolutions per minute. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 5.
TABLE 5
Example 6
At 30 ℃, the pressure of water glass and a sulfuric acid pump flow tube is 0.8Mpa, high-purity water glass 15L with the flow rate of 210L/h, the silicon dioxide concentration of 15wt percent and the modulus of 3.40 and sulfuric acid solution with the flow rate of 40L/h and the concentration of 30wt percent are simultaneously injected into a 50L stirring reaction vessel, 5L of sulfuric acid solution with the flow rate of 40L/h and the concentration of 30wt percent are added for 7min to form silica sol, caustic soda is added to adjust the pH value to 9.0 after the silica sol is formed, the temperature is increased to 90 ℃, KH520 (gamma-glycidoxypropyl) with the silicon dioxide content of 0.40wt percent and KH580 (3-mercaptopropyl trimethoxysilane) with the silicon dioxide content of 0.10wt percent are added, stirring and ageing are carried out for 4h under the conditions, sulfuric acid is added to adjust the pH value to 4 after the ageing is completed, ageing is carried out for 1.0 h, the silica sol is formed, the cooling temperature is 65 ℃ after the gel is completed, the silica sol is pumped into a filter plate frame for water washing, pure water solution with 60% sulfuric acid solution and ammonium bicarbonate according to 55 ℃). Water was 0.10:1, washing the silica gel by pure water at 55 ℃, wherein the washing sequence time interval is 1:5:3:1 respectively, the washing time is 5 hours, the washing time is lower than 50us/cm, after the washing is finished, the silica gel is dispersed for 45 minutes by a dispersing machine and an emulsifying machine, the rotating speed of the dispersing machine is 2500 r/min, and the speed of the emulsifying machine is 4000 r/min. And (3) performing spray drying on the slurry obtained after the dispersion is finished, and performing jet milling to obtain the product with the particle size of 3.00-5.00 mu m.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 6.
TABLE 6
Comparative example 1
The difference from example 1 was that, instead of using high purity water glass, ordinary water glass was used, the elemental analysis of Fe element was equal to 35ppm, al element was equal to 5.3ppm, ca element was equal to 4.7ppm, mg element was equal to 4.9ppm, and the solid water glass was equal to 95.5%, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 7.
TABLE 7
Comparative example 2
The difference compared to example 1 is that instead of using a water glass with pressure and a sulfuric acid flow meter, a common flow tube was used, wherein the water glass flow rate was 200L/h and the sulfuric acid flow rate was 50L/h, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 8.
TABLE 8
Comparative example 3
The difference compared to example 1 is that pure water at 80 ℃ is used instead of pure water at 60 ℃, 50% sulfuric acid solution, ammonium bicarbonate in example 1: the weight ratio of water is 0.05:1, washing the silica gel with pure water at 60 ℃ at a time interval of 1:5:3:1, and directly washing the silica gel for 5 hours, wherein the other steps are the same as those of example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 9.
TABLE 9
Comparative example 4
The difference compared with example 1 is that KH540 (gamma-aminopropyl trimethoxysilane) was added at a silica content of 0.50wt% and KH580 (3-mercaptopropyl trimethoxysilane) was not added, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 10.
Table 10
Comparative example 5
The difference compared with example 1 is that KH580 (3-mercaptopropyl trimethoxysilane) was added at a silica content of 0.50wt% and KH540 (gamma-aminopropyl trimethoxysilane) was not added, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 11.
TABLE 11
Comparative example 6
The difference compared with example 1 is that KH540 (γ -aminopropyl trimethoxysilane) having a silica content of 0.40wt% and A171 (vinyl trimethoxysilane) having a silica content of 0.10wt% were added instead of KH540 (γ -aminopropyl trimethoxysilane) having a silica content of 0.40wt% and KH580 (3-mercaptopropyl trimethoxysilane) having a silica content of 0.10wt% were added, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 12.
Table 12
Comparative example 7
The difference compared with example 1 is that, instead of adding KH540 (γ -aminopropyl trimethoxysilane) having a silica content of 0.40wt% and adding KH580 (3-mercaptopropyl trimethoxysilane) having a silica content of 0.10wt%, KH 171 (vinyl trimethoxysilane) having a silica content of 0.40wt% and adding KH580 (3-mercaptopropyl trimethoxysilane) having a silica content of 0.10wt%, the other operations were the same as those of example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 13.
TABLE 13
Analysis of results
From the detection data of the 6 embodiments of the present invention, it can be seen that the physical indexes of the products produced according to the technical scheme of the present invention are basically close, which indicates that the production of the technical scheme is stable.
It can be seen from comparative example 1 that the oil absorption and the porosity of the product produced by adopting ordinary water glass to replace high-purity water glass are obviously reduced, the bulk density, the conductivity and the iron content are obviously increased, the particle size change is not large, and the degree of the silica sol network structure is reduced mainly because the ordinary water glass hetero element is increased to cause the chelating reaction of the silica primary particles and the hetero element, so that the oil absorption value and the porosity are reduced.
In addition, in the comparative example 2, the conventional common flow tube is adopted to replace the water glass and the sulfuric acid flowmeter with pressure boost, the oil absorption and the porosity of the product are obviously reduced, and the bulk density, the conductivity and the iron content are obviously increased, mainly because the high-pressure convection accelerates the rapid formation of the primary particles of the silicon dioxide, so that the rapid formation of the silicon dioxide network structure is realized, the richness of the silicon dioxide network structure is increased, and the porosity of the silicon dioxide is improved.
In the comparative example 3, the common pure water is directly adopted to replace sulfuric acid solution, ammonium bicarbonate solution and three solutions to wash silica gel, the oil absorption and the porosity of the product are obviously reduced, the bulk density, the conductivity and the iron content are obviously increased, the sulfuric acid solution can reduce the iron content, and the sulfuric acid solution can react with the iron element to a certain extent mainly, so that the iron content in the silicon dioxide structure is reduced; the ammonium ion can ream holes to a certain extent and improve the water washing efficiency, and the main reason is that the ammonium ion can exchange ions with hydrogen ion, so that the porosity of the silicon dioxide is richer and larger, the ammonium bicarbonate can ream holes, and the ammonium ion and the hydrogen ion can exchange to a certain extent and improve the water washing efficiency.
The oil absorption and the porosity of the product synthesized by directly adopting the silane coupling agent A or B in comparative examples 4 and 5 are obviously reduced, the bulk density, the conductivity and the iron content are not greatly changed, but the application effect shared by the two silane coupling agents cannot be achieved, mainly because both the A type (gamma silane coupling agent and the like) and the B type (3-mercaptosilane coupling agent) of the silane coupling agent can react with silicon hydroxyl groups of silicon dioxide, the A type coupling agent can improve the affinity degree of the silicon dioxide particles and the organic polymer, the antistatic property, the lubricating property and the moisture resistance of the silicon dioxide particles, the friction coefficient and the bonding resistance are reduced, the rigidity of the silicon dioxide structure can be improved by the silane coupling agent B, so that silicon dioxide is better dispersed in an opening agent system, and the combination and cooperation of the two can lead the oil absorption and the porosity of the product to be larger, and the silicon dioxide can be better applied to the plastic film opening agent. The synergistic effect of the combined use of the silane coupling agents A and B in the invention is better demonstrated by the comparison of the example 6 and the example 7, while the combined use of the silane coupling agents A-171 (vinyltriethoxysilane) and A-172 (vinyltri (beta-methoxyethoxy) silane) coupling agents can not be expected by replacing the oil absorption and the pore volume of the opening agent synthesized by the silane coupling agent A (gamma silane coupling agent and the like) or B (3-mercaptosilane coupling agent), and the technical effect of the invention can be achieved by screening, scientific and reasonable collocation of the coupling agents A and B is required.
Application Performance test
The three silica sol-gel example products 1-5, 3-5, 5-5 and comparative examples 1-5, 3-5, 5-5 prepared by the invention were compared with Fuji SY340, graies E300 as plastic film opening agent performance applications, polyethylene terephthalate: silica opening agent: dispersant (ethylene glycol): antioxidant (commercially available antioxidant 1010): antistatic agent (sold by Dinghai plastics chemical industry Co., ltd.) according to 93.5:0.5:3:2:1, and then carrying out melt mixing by a double screw extruder, and then carrying out longitudinal stretching, transverse stretching and heat setting treatment to obtain the polyethylene terephthalate film, and carrying out film application performance detection, physical and chemical indexes and application test result data are shown in table 14.
TABLE 14
Compared with Fuji SY340 and Graves E300 opening agent products, the opening agent synthesized by the method has the physical and chemical indexes and application properties close to those of foreign opening agents, even better, has good transparency, lower haze and good transparency, and has opening performance close to those of opening agent products from three samples of examples 1-5, 3-5 and 5-5 and three samples of comparative examples 1-5, 3-5 and 5-5.
It is apparent that the above examples of the present invention are only for clearly illustrating the technical solution of the present invention, and are not limited to the specific embodiments of the present invention. Any modification, equivalent replacement, improvement, etc. that comes within the spirit and principle of the claims of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The preparation method of the sol-gel film opening agent is characterized by comprising the following steps:
s1, forming silica sol by pressurizing and convection of a water glass solution and sulfuric acid;
s2, heating the silica sol obtained in the step S1, adjusting the pH to be alkaline, then adding a silane coupling agent A and a silane coupling agent B for modification, adjusting the pH to be acidic after aging, and then aging to form silica gel;
s3, washing the silica gel obtained in the step S2, and uniformly dispersing the washed silica gel;
s4, drying and crushing the slurry after the dispersion in the step S3 to obtain the slurry;
the silane coupling agent A is one of gamma-aminopropyl methyl diethoxy silane, gamma-aminopropyl methyl dimethoxy silane, gamma-aminopropyl trimethoxy silane, gamma-aminopropyl triethoxy silane, gamma-glycidol ether oxypropyl and gamma- (methacryloyloxy) propyl trimethoxy silane, and the silane coupling agent B is one of 3-mercaptopropyl trimethoxy silane and 3-mercaptopropyl triethoxy silane.
2. The method for preparing a sol-gel film opening agent according to claim 1, wherein the silica modulus of the water glass solution in the step S1 is 3.20-3.40, the concentration is 10-20 wt%, and the sulfuric acid concentration is 30-50 wt%.
3. The method for preparing the sol-gel film opening agent according to claim 1, wherein the water glass solution in the step S1 has the Fe element content of less than or equal to 15ppm, the Al element content of less than or equal to 1ppm, the Ca element content of less than or equal to 1ppm, the Mg element content of less than or equal to 1ppm, and the solid water glass solubility of more than or equal to 99.5%.
4. The method for preparing the sol-gel film opening agent according to claim 1, wherein the flow pipeline pressure of the pressurized water glass and sulfuric acid in the step S1 is kept at 0.5 Mpa-1 Mpa, the flow rate of the water glass solution is 180L/h-230L/h, and the flow rate of the sulfuric acid is 30L/h-50L/h.
5. The method for preparing the sol-gel film opening agent according to claim 1, wherein the total addition amount of the silane coupling agent in the step S2 is 0.50-0.80 wt% of the dry base material, and the mass ratio of the silane coupling agent A to the silane coupling agent B is 4:1.
6. The method for preparing a sol-gel film opening agent according to claim 1, wherein the washing in step S3 is to wash with pure water, sulfuric acid solution, ammonium salt aqueous solution, and pure water at a time interval of 1:5:3:1, respectively, until the conductivity of the silica gel is 50us/cm or less.
7. The method for preparing the sol-gel film opening agent according to claim 6, wherein the conductivity of the pure water is lower than 5us/cm, the temperature is 50-80 ℃, the concentration of the sulfuric acid solution is 30-60%, the ammonium salt is one of ammonium sulfate, ammonium bisulfate, ammonium carbonate and ammonium bicarbonate, and the weight ratio of the ammonium salt to water in the ammonium salt aqueous solution is 0.05-0.10: 1.
8. the method for preparing a sol-gel film opening agent according to claim 1, wherein in the step S3, the dispersion is performed under the combined action of a dispersing machine and an emulsifying machine, the rotation degree of the dispersing machine is 1500-2500 rpm, the rotation degree of the emulsifying machine is 3000-5000 rpm, and the combined action time is 30-60 minutes.
9. A sol-gel film opener prepared by the method of any one of claims 1-8, wherein the film opener has a particle size of 3.00-5.00 μm.
10. Use of the film opener of claim 9 for improving the properties of a polyethylene terephthalate film.
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