CN114634635A - Composite spherical polydimethylsiloxane, preparation method thereof and composition using composite spherical polydimethylsiloxane - Google Patents
Composite spherical polydimethylsiloxane, preparation method thereof and composition using composite spherical polydimethylsiloxane Download PDFInfo
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- -1 polydimethylsiloxane Polymers 0.000 title claims abstract description 226
- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 177
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title claims abstract description 177
- 239000002131 composite material Substances 0.000 title claims abstract description 113
- 239000000203 mixture Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 36
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 59
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 49
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 24
- 229960000686 benzalkonium chloride Drugs 0.000 claims abstract description 16
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims abstract description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 60
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 22
- 239000003085 diluting agent Substances 0.000 claims description 20
- 239000000839 emulsion Substances 0.000 claims description 20
- 239000004005 microsphere Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 16
- 238000006482 condensation reaction Methods 0.000 claims description 16
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 12
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 9
- 239000012895 dilution Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229920000768 polyamine Polymers 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 2
- 241000195493 Cryptophyta Species 0.000 abstract description 7
- 230000001954 sterilising effect Effects 0.000 abstract description 7
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 description 19
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000005764 inhibitory process Effects 0.000 description 6
- 230000001877 deodorizing effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000003899 bactericide agent Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009967 tasteless effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/02—Odour removal or prevention of malodour
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/08—Corrosion inhibition
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/04—Surfactants, used as part of a formulation or alone
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses composite spherical polydimethylsiloxane, a preparation method thereof and a composition using the same, and relates to the technical field of polydimethylsiloxane. The invention discloses composite spherical polydimethylsiloxane, which is prepared by condensing a polydimethylsiloxane prepolymer and polysiloxane oligomer with a main chain containing a benzene ring structure. The composite spherical polydimethylsiloxane is compounded with polysiloxane oligomer with a benzene ring structure in a main chain through a polydimethylsiloxane prepolymer, the rigidity of the main chain is improved due to the benzene ring structure on the main chain, so that the heat resistance of the composite spherical polydimethylsiloxane is obviously improved, and a cationic surfactant prepared from benzalkonium chloride solution is added on the surface of the composite spherical polydimethylsiloxane, so that the sterilization and algae killing capabilities of the composite spherical polydimethylsiloxane are improved.
Description
Technical Field
The invention relates to the technical field of polydimethylsiloxane, in particular to composite spherical polydimethylsiloxane, a preparation method thereof and a composition using the same.
Background
The dimethyl silicone oil in the chemical state of the polydimethylsiloxane is a liquid or silica gel with the appearance from colorless and transparent volatile liquid to extremely high viscosity according to the difference of relative molecular mass, is tasteless, has high transparency, heat resistance, cold resistance, small change of viscosity along with temperature, waterproofness, small surface tension and thermal conductivity, has the thermal conductivity coefficient of 0.134-0.159W/(m.K), the light transmittance is 100 percent, and the dimethyl silicone oil is nontoxic, tasteless, physiologically inert and good in chemical stability. Good electric insulation, weather resistance and hydrophobicity, and high shear resistance, and can be used for a long time at the temperature of minus 50 ℃ to 200 ℃. The composite material has excellent physical characteristics, can be directly used for damp-proof insulation, damping, shock absorption, defoaming, lubrication, polishing and the like, and can be widely used as insulation lubrication, shock prevention, oil dust prevention, dielectric fluid and heat carriers. And as defoamers, release agents, paints and commodity additives.
Chinese patent CN102746528B discloses a method for preparing polydimethylsiloxane porous pellets, which comprises the following steps: 1) taking 100 parts by weight of polydimethylsiloxane prepolymer, and adding 60-120 parts by weight of diluent for dilution, wherein the diluent is one or a mixed solution of carbon tetrachloride and n-octane; 2) adding 2-4 parts by weight of curing agent into the diluted polydimethylsiloxane prepolymer obtained in the step 1), and stirring and mixing uniformly; 3) dropwise adding the mixed solution obtained in the step 2) into a surfactant solution, stirring and reacting at the temperature of 50-100 ℃ at the stirring speed of 50-100r/min, fishing out and washing after the reaction is finished to obtain the polydimethylsiloxane pellets with the porous structure. The porous small ball prepared by the method can float on the water surface, is convenient for effectively absorbing the organic solvent spread on the water surface, has larger specific surface area, and greatly improves the oil absorption and the oil absorption speed.
Although this application solves the problems in the background art to some extent, the following problems exist in this application: 1. the buoyancy of the material is increased by arranging the small holes, but the heat resistance of the material is not enhanced, so that the oil cannot be adsorbed when the oil is burnt on the water surface; 2. only oil stains are adsorbed to play a role in purifying water, but the water body cannot be disinfected, and the water purifying capacity is limited.
Disclosure of Invention
The invention aims to provide composite spherical polydimethylsiloxane, a preparation method thereof and a composition using the same, wherein the composite spherical polydimethylsiloxane is prepared by compounding polysiloxane oligomer with a main chain containing a benzene ring structure through a polydimethylsiloxane prepolymer to prepare the composite spherical polydimethylsiloxane with the main chain containing the benzene ring structure, the rigidity of the main chain is improved due to the benzene ring structure on the main chain, so that the heat resistance of the composite spherical polydimethylsiloxane is obviously improved, a cationic surfactant prepared from benzalkonium chloride solution is added on the surface of the composite spherical polydimethylsiloxane, the sterilization and algae killing capability of the composite spherical polydimethylsiloxane is improved, and the composite spherical polydimethylsiloxane has certain deoiling, deodorizing and corrosion inhibition functions, has a good effect on purifying water sources, contains the benzene ring structure on the main chain of benzalkonium chloride per se, and improves the heat resistance of the surface of the composite spherical polydimethylsiloxane, to solve the problems set forth in the background art described above.
In order to achieve the purpose, the invention provides the following technical scheme: the composite spherical polydimethylsiloxane is prepared by condensing a polydimethylsiloxane prepolymer and polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the polydimethylsiloxane with the main chain containing the benzene ring structure, composite spherical shape and a microporous structure.
The invention aims to solve another technical problem of providing a preparation method of composite spherical polydimethylsiloxane, which comprises the following steps:
s1: preparing polysiloxane oligomer with a main chain containing a benzene ring structure;
s2: performing condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare composite polydimethylsiloxane;
s3: diluting the composite polydimethylsiloxane by adding a diluent, adding a curing agent into the diluent after dilution, stirring and mixing uniformly, and exhausting air;
s4: adding a cationic surfactant into the obtained mixed solution, reacting, and stirring at a stirring speed of 50-100r/min at 20-25 ℃ to react to form polydimethylsiloxane emulsion microspheres;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
Preferably, the S1 includes the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding 10-12 parts by weight of dimethyl dimethoxysilane into the solution containing the benzene-based monomer, 5-12 parts by weight of water and 10-18 parts by weight of dimethyl dimethoxysilane;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 80-120 ℃ to react for 8-10h in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 6-7, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
Preferably, the S2 includes the following steps:
s21: dissolving 2-10 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 15-30 parts by weight of polydimethylsiloxane prepolymer in acetone, and adding 0.1-0.8 part by weight of catalyst;
s22: introducing nitrogen, reacting for 6-8h at 40-80 ℃ in nitrogen atmosphere, adjusting the pH value to 6-7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
Preferably, the cationic surfactant is benzalkonium chloride solution, and the concentration of the solution is 0.5-15 wt%.
Preferably, the curing temperature in S5 is required to be higher than the three-phase equilibrium point, and the curing time is 3-48 hours.
Preferably, the method is characterized in that: the diluent is carbon tetrachloride and n-octane in a ratio of 1: 1, and mixing the obtained mixed solution.
Preferably, it is characterized in that: the curing agent is at least one of polyalkoxysilane, polyamine silane, polyamido silane or hydrogen-containing silicone oil.
The invention aims to solve another technical problem of providing a preparation method of composite spherical polydimethylsiloxane, which comprises the following steps:
the first step is as follows: preparing polysiloxane oligomer with a main chain containing a benzene ring structure;
the second step is that: performing condensation reaction on the polydimethylsiloxane prepolymer and polysiloxane oligomer with a main chain containing a benzene ring structure to prepare composite polydimethylsiloxane;
the third step: adding a curing agent into the composite polydimethylsiloxane, stirring and mixing uniformly, allowing gas to enter during stirring, and controlling the stirring temperature to be 30-50 ℃;
the fourth step: adding a cationic surfactant into the obtained mixed solution, reacting, and stirring at a stirring speed of 50-100r/min at 20-25 ℃ to react to form polydimethylsiloxane emulsion microspheres;
the fifth step: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
Another technical problem to be solved by the present invention is to provide a composition comprising composite spherical polydimethylsiloxane.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the composite spherical polydimethylsiloxane, the preparation method and the composition using the composite spherical polydimethylsiloxane, disclosed by the invention, the composite spherical polydimethylsiloxane is prepared by compounding the polydimethylsiloxane prepolymer with the polysiloxane oligomer with the main chain containing the benzene ring structure, so that the rigidity of the main chain is improved, and the heat resistance of the composite spherical polydimethylsiloxane is obviously improved;
2. according to the composite spherical polydimethylsiloxane, the preparation method and the composition using the composite spherical polydimethylsiloxane, the cationic surfactant prepared from benzalkonium chloride solution is added on the surface of the composite spherical polydimethylsiloxane, so that the sterilization and algae removal capabilities of the composite spherical polydimethylsiloxane are improved, and the composite spherical polydimethylsiloxane has certain oil removal and deodorization capabilities and a corrosion inhibition effect and has a good effect on water source purification;
3. according to the composite spherical polydimethylsiloxane, the preparation method and the composition using the composite spherical polydimethylsiloxane, the main chain of benzalkonium chloride also contains a benzene ring structure, so that the heat resistance of the surface of the composite spherical polydimethylsiloxane is improved.
Drawings
FIG. 1 is a flow chart of the preparation of composite spherical polydimethylsiloxane of the present invention;
FIG. 2 is a flow chart of the present invention for preparing a polysiloxane oligomer having a main chain containing a phenyl ring structure;
FIG. 3 is a flow chart of the preparation of composite polydimethylsiloxane of the present invention;
FIG. 4 is a flow chart of another embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The composite spherical polydimethylsiloxane is prepared by condensing a polydimethylsiloxane prepolymer and polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the polydimethylsiloxane with the main chain containing the benzene ring structure, composite spherical shape and a microporous structure.
The first embodiment is as follows:
referring to fig. 1 to 3, in order to better show the preparation method of the composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of the composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding dimethyldimethoxysilane into the solution containing the benzene-based monomer, wherein the benzene monomer is 10 parts by weight, the water is 5 parts by weight, and the dimethyldimethoxysilane is 10 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 80 ℃ to react for 8 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 6, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: dissolving 2 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 15 parts by weight of polydimethylsiloxane prepolymer in acetone, and adding 0.1 part by weight of catalyst;
s22: introducing nitrogen, reacting for 6h at 40 ℃ in nitrogen atmosphere, adjusting the pH value to 6, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a diluent into the composite polydimethylsiloxane for dilution, wherein the diluent is prepared from carbon tetrachloride and n-octane according to the weight ratio of 1: 1, adding a curing agent into the diluent after dilution, wherein the curing agent is at least one of polyalkoxysilane, polyamine silane, polyamido silane or hydrogen-containing silicone oil, stirring and mixing uniformly, exhausting air, and pumping out the air through a vacuum pump to prevent the gas from entering and influencing the surface integrity of the composite polydimethylsiloxane;
s4: adding a cationic surfactant into the obtained mixed solution for reaction, and stirring at a stirring speed of 50r/min at 20 ℃ for reaction to form polydimethylsiloxane emulsion microspheres, wherein the cationic surfactant is benzalkonium chloride solution, the concentration of the solution is 0.5 wt%, and benzalkonium chloride is a cationic surfactant, belongs to a non-oxidative bactericide, has broad-spectrum and high-efficiency sterilization and algae-killing capability, can effectively control the propagation of bacteria and algae and the growth of slime in water, has good slime stripping effect and certain dispersion and permeation effects, has certain deoiling, deodorizing and corrosion inhibition effects, and has a good effect on purifying water sources;
s5: heating and completely curing the prepared polydimethylsiloxane emulsion microspheres, and drying to obtain spherical polydimethylsiloxane with a labyrinth or dimple-shaped fold structure on the surface, wherein the curing temperature is higher than the three-phase equilibrium point, and the curing time is 3 hours;
example two:
referring to fig. 1 to 3, in order to better show the preparation method of the composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of the composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding dimethyldimethoxysilane into the solution containing the phenyl monomer, wherein the benzene monomer is 12 parts by weight, the water is 12 parts by weight, and the dimethyldimethoxysilane is 18 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 120 ℃ to react for 10 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: dissolving 10 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 30 parts by weight of polydimethylsiloxane prepolymer into acetone, and adding 0.8 part by weight of catalyst;
s22: introducing nitrogen, reacting at 80 ℃ for 8h in nitrogen atmosphere, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a diluent into the composite polydimethylsiloxane for dilution, wherein the diluent is prepared from carbon tetrachloride and n-octane according to the weight ratio of 1: 1, adding a curing agent into the diluent after dilution, wherein the curing agent is at least one of polyalkoxysilane, polyamine silane, polyamido silane or hydrogen-containing silicone oil, stirring and mixing uniformly, exhausting air, and pumping out the air through a vacuum pump to prevent the gas from entering and influencing the surface integrity of the composite polydimethylsiloxane;
s4: adding a cationic surfactant into the obtained mixed solution for reaction, and stirring at a stirring speed of 100r/min at 25 ℃ for reaction to form polydimethylsiloxane emulsion microspheres, wherein the cationic surfactant is benzalkonium chloride solution, the concentration of the solution is 15 wt%, and benzalkonium chloride is a cationic surfactant, belongs to a non-oxidative bactericide, has broad-spectrum and high-efficiency sterilization and algae-killing capability, can effectively control the propagation and slime growth of bacteria and algae in water, has good slime stripping effect and certain dispersion and permeation effects, has certain deoiling, deodorizing and corrosion inhibition effects, and has a good effect on purifying water sources;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain spherical polydimethylsiloxane with a labyrinth or dimple-shaped fold structure on the surface, wherein the curing temperature is higher than the three-phase equilibrium point, and the curing time is 48 hours.
Example three:
referring to fig. 1 to 3, in order to better show the preparation method of the composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of the composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding dimethyl dimethoxy silane into the solution containing the benzene-based monomer, wherein the benzene monomer is 10 parts by weight, the water is 5 parts by weight, and the dimethyl dimethoxy silane is 18 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 100 ℃ to react for 8 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 6, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: dissolving 5 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 20 parts by weight of polydimethylsiloxane prepolymer in acetone, and adding 0.5 part by weight of catalyst;
s22: introducing nitrogen, reacting for 7h at 60 ℃ in a nitrogen atmosphere, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a diluent into the composite polydimethylsiloxane for dilution, wherein the diluent is prepared from carbon tetrachloride and n-octane according to the weight ratio of 1: 1, adding a curing agent into the diluent after dilution, wherein the curing agent is at least one of polyalkoxysilane, polyamine silane, polyamido silane or hydrogen-containing silicone oil, stirring and mixing uniformly, exhausting air, and pumping out the air through a vacuum pump to prevent the gas from entering and influencing the surface integrity of the composite polydimethylsiloxane;
s4: adding a cationic surfactant into the obtained mixed solution for reaction, and stirring at a stirring speed of 100r/min at 20 ℃ for reaction to form polydimethylsiloxane emulsion microspheres, wherein the cationic surfactant is benzalkonium chloride solution, the concentration of the solution is 10 wt%, and benzalkonium chloride is a cationic surfactant, belongs to a non-oxidative bactericide, has broad-spectrum and high-efficiency sterilization and algae-killing capability, can effectively control the propagation and slime growth of bacteria and algae in water, has good slime stripping effect and certain dispersion and permeation effects, has certain deoiling, deodorizing and corrosion inhibition effects, and has a good effect on purifying water sources;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then are dried to obtain spherical polydimethylsiloxane with a labyrinth or dimple-shaped folded structure on the surface, the curing temperature is higher than the three-phase equilibrium point, and the curing time is 24 hours.
Example four
Referring to fig. 2 to 4, in order to better show the preparation method of composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding dimethyldimethoxysilane into the solution containing the benzene-based monomer, wherein the benzene monomer is 10 parts by weight, the water is 5 parts by weight, and the dimethyldimethoxysilane is 10 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 80-120 ℃ to react for 8 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 6, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: dissolving 2 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 15 parts by weight of polydimethylsiloxane prepolymer in acetone, and adding 0.1 part by weight of catalyst;
s22: introducing nitrogen, reacting for 6h at 40 ℃ in nitrogen atmosphere, adjusting the pH value to 6, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a curing agent into the composite polydimethylsiloxane, stirring and mixing uniformly, allowing gas to enter during stirring, wherein the stirring temperature is 30 ℃, and allowing the gas to enter the composite polydimethylsiloxane so that micropores appear on the surface of the composite polydimethylsiloxane and the same effect as pore-forming of a diluent is realized;
s4: adding a cationic surfactant into the obtained mixed solution, wherein the concentration of the solution is 0.5 wt%, reacting, and stirring at a stirring speed of 50r/min at 20 ℃ for reaction to form polydimethylsiloxane emulsion microspheres;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
EXAMPLE five
Referring to fig. 2 to 4, in order to better show the preparation method of composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding dimethyldimethoxysilane into the solution containing the phenyl monomer, wherein the benzene monomer is 12 parts by weight, the water is 12 parts by weight, and the dimethyldimethoxysilane is 18 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 120 ℃ to react for 10 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: dissolving 10 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 30 parts by weight of polydimethylsiloxane prepolymer into acetone, and adding 0.8 part by weight of catalyst;
s22: introducing nitrogen, reacting at 80 ℃ for 8h in nitrogen atmosphere, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a curing agent into the composite polydimethylsiloxane, stirring and mixing uniformly, allowing gas to enter during stirring, wherein the stirring temperature is 50 ℃, and allowing the gas to enter the composite polydimethylsiloxane so that micropores appear on the surface of the composite polydimethylsiloxane and the same effect as pore-forming of a diluent is realized;
s4: adding a cationic surfactant into the obtained mixed solution, wherein the concentration of the solution is 15 wt%, reacting, and stirring at a stirring speed of 100r/min at 25 ℃ to react to form polydimethylsiloxane emulsion microspheres;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
EXAMPLE six
Referring to fig. 2 to 4, in order to better show the preparation method of composite spherical polydimethylsiloxane, the present embodiment provides a preparation method of composite spherical polydimethylsiloxane, which includes the following steps:
s1: the preparation method of the polysiloxane oligomer with the main chain containing the benzene ring structure specifically comprises the following steps:
s11: dissolving a benzene monomer in water, and slowly dropwise adding dimethyldimethoxysilane into the solution containing the benzene-based monomer, wherein the benzene monomer is 10 parts by weight, the water is 10 parts by weight, and the dimethyldimethoxysilane is 18 parts by weight;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 100 ℃ to react for 8 hours in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
S2: the preparation method comprises the following steps of carrying out condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare the composite polydimethylsiloxane, wherein the condensation reaction comprises the following steps:
s21: taking 5 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 20 parts by weight of polydimethylsiloxane prepolymer, dissolving the polysiloxane oligomer and the polydimethylsiloxane prepolymer in acetone, and adding 0.5 part by weight of catalyst;
s22: introducing nitrogen, reacting for 8h at 60 ℃ in a nitrogen atmosphere, adjusting the pH value to 7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
S3: adding a curing agent into the composite polydimethylsiloxane, stirring and mixing uniformly, allowing gas to enter during stirring, wherein the stirring temperature is 50 ℃, and allowing the gas to enter the composite polydimethylsiloxane so that micropores appear on the surface of the composite polydimethylsiloxane and the same effect as pore-forming of a diluent is realized;
s4: adding a cationic surfactant into the obtained mixed solution, wherein the concentration of the solution is 10 wt%, reacting, and stirring at a stirring speed of 100r/min at 25 ℃ to react to form polydimethylsiloxane emulsion microspheres;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
Six samples, namely, example one, example two, example three, example four, example five and example six, were prepared from the above examples, respectively, while the components of the cationic surfactant were changed without adding a polysiloxane oligomer having a benzene ring in the main chain in the comparative example to prepare comparative example one and comparative example two, and the following data were obtained by comparing with the comparative examples.
From the above table, it can be seen that the composite spherical polydimethylsiloxane obtained in the first to sixth embodiments, in which the polysiloxane oligomer having a benzene ring in the main chain is added, has good heat resistance and can be applied to a high-temperature environment, and the cationic surfactant adopts benzalkonium chloride solution, so that a bacteriostatic effect can be achieved.
In summary, the following steps: the composite spherical polydimethylsiloxane is prepared by compounding polydimethylsiloxane prepolymer with polysiloxane oligomer with a main chain containing a benzene ring structure, the rigidity of the main chain is improved due to the benzene ring structure on the main chain, so that the heat resistance of the composite spherical polydimethylsiloxane is obviously improved, a cationic surfactant prepared from benzalkonium chloride solution is added on the surface of the composite spherical polydimethylsiloxane, the sterilization and algae killing capabilities of the composite spherical polydimethylsiloxane are improved, meanwhile, the composite spherical polydimethylsiloxane has certain deoiling, deodorizing and corrosion inhibition functions, and has a good effect on water purification, the main chain of benzalkonium chloride also contains the benzene ring structure, and the heat resistance of the surface of the composite spherical polydimethylsiloxane is improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. The composite spherical polydimethylsiloxane is characterized in that: and condensing the polydimethylsiloxane prepolymer and polysiloxane oligomer with a main chain containing a benzene ring structure to obtain the polydimethylsiloxane with a main chain containing a benzene ring structure composite sphere and a microporous structure.
2. The method for preparing composite spherical polydimethylsiloxane of claim 1, which comprises the following steps:
s1: preparing polysiloxane oligomer with a main chain containing a benzene ring structure;
s2: performing condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare composite polydimethylsiloxane;
s3: diluting the composite polydimethylsiloxane by adding a diluent, adding a curing agent into the diluent after dilution, stirring and mixing uniformly, and exhausting air;
s4: adding a cationic surfactant into the obtained mixed solution for reaction, and stirring at the stirring speed of 50-100r/min at the temperature of 20-25 ℃ for reaction to form polydimethylsiloxane emulsion microspheres;
s5: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
3. The method for preparing composite spherical polydimethylsiloxane according to claim 2, wherein the composite spherical polydimethylsiloxane comprises the following steps: the S1 includes the steps of:
s11: adding benzene monomer into water for dissolving, and slowly dropwise adding 10-12 parts by weight of dimethyl dimethoxysilane into the solution containing the benzene-based monomer, 5-12 parts by weight of water and 10-18 parts by weight of dimethyl dimethoxysilane;
s12: adding a proper amount of catalyst, introducing nitrogen, and heating to 80-120 ℃ to react for 8-10h in a nitrogen environment;
s13: after the reaction is finished, adjusting the pH value to 6-7, removing inorganic matters, and removing the solvent under reduced pressure to obtain the polysiloxane oligomer with the main chain containing benzene rings.
4. The method for preparing composite spherical polydimethylsiloxane as claimed in claim 2, wherein the method comprises the following steps: the S2 includes the steps of:
s21: taking 2-10 parts by weight of polysiloxane oligomer with a benzene ring-containing main chain and 15-30 parts by weight of polydimethylsiloxane prepolymer, dissolving the polysiloxane oligomer and the polydimethylsiloxane prepolymer in acetone, and adding 0.1-0.8 part by weight of catalyst;
s22: introducing nitrogen, reacting for 6-8h at 40-80 ℃ in nitrogen atmosphere, adjusting the pH value to 6-7, removing inorganic matters, and removing the solvent under reduced pressure after the reaction is finished to obtain the composite polydimethylsiloxane.
5. The method for preparing composite spherical polydimethylsiloxane as claimed in claim 2, wherein the method comprises the following steps: the cationic surfactant is benzalkonium chloride solution with concentration of 0.5-15 wt%.
6. The method for preparing composite spherical polydimethylsiloxane according to claim 2, wherein the composite spherical polydimethylsiloxane comprises the following steps: the curing temperature in the S5 is required to be higher than the three-phase equilibrium point, and the curing time is 3-48 hours.
7. The method for preparing composite spherical polydimethylsiloxane according to claim 2, wherein the composite spherical polydimethylsiloxane comprises the following steps: the diluent is prepared from carbon tetrachloride and n-octane in a proportion of 1: 1 by volume ratio of the resulting mixture.
8. The method for preparing composite spherical polydimethylsiloxane according to claim 2, wherein the composite spherical polydimethylsiloxane comprises the following steps: the curing agent is at least one of polyalkoxysilane, polyamine silane, polyamido silane or hydrogen-containing silicone oil.
9. The method for preparing composite spherical polydimethylsiloxane according to claim 2, wherein the composite spherical polydimethylsiloxane comprises the following steps: further comprising the steps of:
the first step is as follows: preparing polysiloxane oligomer with a main chain containing a benzene ring structure;
the second step is that: performing condensation reaction on a polydimethylsiloxane prepolymer and a polysiloxane oligomer with a main chain containing a benzene ring structure to prepare composite polydimethylsiloxane;
the third step: adding a curing agent into the composite polydimethylsiloxane, stirring and mixing uniformly, allowing gas to enter during stirring, and controlling the stirring temperature to be 30-50 ℃;
the fourth step: adding a cationic surfactant into the obtained mixed solution, reacting, and stirring at a stirring speed of 50-100r/min at 20-25 ℃ to react to form polydimethylsiloxane emulsion microspheres;
the fifth step: the prepared polydimethylsiloxane emulsion microspheres are heated and cured completely, and then dried to obtain the spherical polydimethylsiloxane with the labyrinth or dimple-shaped folded structure on the surface.
10. A composition characterized by: comprising the composite spherical polydimethylsiloxane prepared according to any of claims 2-9.
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