CN110258112A - A kind of high-performance flexible agent - Google Patents
A kind of high-performance flexible agent Download PDFInfo
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- CN110258112A CN110258112A CN201910635175.2A CN201910635175A CN110258112A CN 110258112 A CN110258112 A CN 110258112A CN 201910635175 A CN201910635175 A CN 201910635175A CN 110258112 A CN110258112 A CN 110258112A
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- Prior art keywords
- silicone oil
- amino silicone
- performance flexible
- hydrophilic amino
- added
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- 229920000570 polyether Polymers 0.000 claims abstract description 65
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229920013822 aminosilicone Polymers 0.000 claims abstract description 43
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 36
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 22
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- NAPSCFZYZVSQHF-UHFFFAOYSA-N dimantine Chemical compound CCCCCCCCCCCCCCCCCCN(C)C NAPSCFZYZVSQHF-UHFFFAOYSA-N 0.000 claims abstract description 17
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims abstract description 15
- FSKTVLIDJTYDMW-UHFFFAOYSA-N [amino(methoxy)silyl]oxymethane Chemical compound CO[SiH](N)OC FSKTVLIDJTYDMW-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 silicon quaternary ammonium salt Chemical class 0.000 claims abstract description 7
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 20
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 19
- 230000015572 biosynthetic process Effects 0.000 claims description 15
- 238000003786 synthesis reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 35
- 239000004744 fabric Substances 0.000 abstract description 8
- 239000004902 Softening Agent Substances 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 230000000845 anti-microbial effect Effects 0.000 abstract description 3
- 238000004332 deodorization Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 229920002545 silicone oil Polymers 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- VMMIGBGQMPISJP-UHFFFAOYSA-N aminosilyloxymethane Chemical compound CO[SiH2]N VMMIGBGQMPISJP-UHFFFAOYSA-N 0.000 description 3
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000012296 anti-solvent Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036299 sexual function Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to softening agent technical fields, especially a kind of high-performance flexible agent, including following component: chloropropyl triethoxysilane, octamethylcy-clotetrasiloxane, dimethoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide, it is chloropropyl triethoxysilane 3-6% according to weight percent, octamethylcy-clotetrasiloxane 50-60%, dimethoxy amino silane 5-10%, active polyether 10-20%, tetramethylammonium hydroxide 0.1-0.5%, octadecyldimethyl ammonia 10-20%, isopropanol 12-15%, potassium iodide is a small amount of, polyethers hydrophilic amino silicone oil is for improving fabric feeling in the high-performance flexible agent, hydrophilic organic silicon quaternary ammonium salt provides anti-microbial property, so that antibacterial fabric deodorization, then polyethers hydrophilic ammonia Base silicone oil, polyethers hydrophilic amino silicone oil are mixed according to appropriate proportioning, and the two synergistic effect effectively raises antibacterial and softness.
Description
Technical field
The present invention relates to softening agent technical field more particularly to a kind of high-performance flexible agent.
Background technique
Softening agent is a kind of quiet, dynamic friction coefficient chemical substance that can change fiber.When change, feel touch has flat
Sliding sense, is easy to move on fiber or fabric；When changing dynamic friction coefficient, the fine structure between fiber and fiber is easy to phase
It is mutually mobile, that is, fiber or fabric it is easily deformable.The comprehensive of the two feels to be exactly soft.Softening agent is had as ionic to divide
Cationic, non-ionic, anionic and four kinds of both sexes quaternary.But existing softening agent performance is single, Bu Nengyou
Effect carries out antimicrobial treatment for textile fabric.
Summary of the invention
The purpose of the present invention is to solve existing in the prior art, softening agent sexual function is single, the disadvantage of performance deficiency,
And a kind of high-performance flexible agent proposed.
To achieve the goals above, present invention employs following technical solutions:
Design a kind of high-performance flexible agent, including following component: chloropropyl triethoxysilane, four silicon oxygen of prestox ring
Alkane, dimethoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide, according to
Weight percent is chloropropyl triethoxysilane 3-6%, octamethylcy-clotetrasiloxane 50-60%, dimethoxy amino silane 5-
10%, active polyether 10-20%, tetramethylammonium hydroxide 0.1-0.5%, octadecyldimethyl ammonia 10-20%, isopropanol
12-15%, potassium iodide are a small amount of.
Preferably, the purity of the chloropropyl triethoxysilane is 98 percent.
Preferably, the preparation of the high-performance flexible agent includes the following steps:
The synthesis of S1, organosilicon quaternary ammonium salt, in four mouthfuls equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Octadecyldimethyl ammonia, isopropanol, chloropropyl triethoxysilane are sequentially added according to said ratio in flask, head is passed through nitrogen
Gas is stirred at low speed, and heating temperature is 80-90 DEG C, and in reflux temperature successive reaction 20-30h, then filtering solution is removed not
Solvent and unreacted reactant are held in soluble antioxidant residue, finally vacuum distillation recycling, finally obtain in golden yellow organosilicone quaternary ammonium
Salt；
The synthesis of S2, polyethers hydrophilic amino silicone oil are being equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Four-hole boiling flask according to said ratio be added octamethylcy-clotetrasiloxane, then carry out heating stir at low speed, control temperature exist
100-115 DEG C, tetramethylammonium hydroxide then is added as catalyst according to said ratio, then continuous heating keeps the temperature 30-
45min is added dimethoxy amino silane as coupling agent according to said ratio after waiting its viscosity to significantly increase, controls temperature and exist
Polyethers hydrophilic amino silicone oil is obtained after 100-115 DEG C of continuous heating heat preservation 3-6h；
The synthesis of S3, polyether-containing aminopolysiloxane, equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
The polyethers hydrophilic amino silicone oil for preparing in S2 is added in four-hole boiling flask, isopropanol then is added according to said ratio, then plus
Heat heat preservation carries out back flow reaction between 80-90 DEG C, until reactant is transparent subsequent continuation of insurance temperature 3-4h, is finally depressurized
Distillation sloughs isopropanol and obtains polyether-containing aminopolysiloxane；
S4, high-performance flexible agent mixture, by organosilicon quaternary ammonium salt obtained above, polyethers hydrophilic amino silicone oil and
Polyethers hydrophilic amino silicone oil, which is added in mixing plant, uniformly to be mixed, and is according to the weight ratio organosilicon quaternary ammonium salt:
Polyethers hydrophilic amino silicone oil: then polyethers hydrophilic amino silicone oil 1:2:2 carries out high speed dispersion stirring until obtaining light yellow
The preparation of thick liquid completion high-performance flexible agent.
Preferably, micro dilution liquor kalii iodide is additionally added in the step S1 as antioxidant.
Preferably, control pressure is 0.01 between 0.04MPa when being evaporated under reduced pressure in step S1, S3.
A kind of high-performance flexible agent proposed by the present invention, beneficial effect are: containing organosilicon in the high-performance flexible agent
Quaternary ammonium salt, polyethers hydrophilic amino silicone oil, polyethers hydrophilic amino silicone oil, polyethers hydrophilic amino silicone oil is for improving fabric hand
Sense, hydrophily make fabric more comfortable soft, and organosilicon quaternary ammonium salt provides anti-microbial property, so that antibacterial fabric deodorization, so
Polyethers hydrophilic amino silicone oil, polyethers hydrophilic amino silicone oil are mixed according to appropriate proportioning afterwards, and the two synergistic effect effectively mentions
High antibacterial and softness.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment one
A kind of high-performance flexible agent, including following component: chloropropyl triethoxysilane, octamethylcy-clotetrasiloxane, two
Methoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide, according to weight
Percentage is chloropropyl triethoxysilane 3%, octamethylcy-clotetrasiloxane 50%, dimethoxy amino silane 5%, active polyether
10%, tetramethylammonium hydroxide 0.1%, octadecyldimethyl ammonia 10%, isopropanol 12%, potassium iodide is a small amount of, chloropropyl three
The purity of Ethoxysilane is 98 percent.
The preparation of high-performance flexible agent includes the following steps:
The synthesis of S1, organosilicon quaternary ammonium salt, in four mouthfuls equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Octadecyldimethyl ammonia, isopropanol, chloropropyl triethoxysilane are sequentially added according to said ratio in flask, head is passed through nitrogen
Gas is stirred at low speed, and heating temperature is 80-90 DEG C, and in reflux temperature successive reaction 20-30h, then filtering solution is removed not
Solvent and unreacted reactant are held in soluble antioxidant residue, finally vacuum distillation recycling, finally obtain in golden yellow organosilicone quaternary ammonium
Salt is eventually adding micro dilution liquor kalii iodide as antioxidant, and control pressure is in 0.01MPa；
The synthesis of S2, polyethers hydrophilic amino silicone oil are being equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Four-hole boiling flask according to said ratio be added octamethylcy-clotetrasiloxane, then carry out heating stir at low speed, control temperature exist
100 DEG C, tetramethylammonium hydroxide then is added as catalyst according to said ratio, then continuous heating keeps the temperature 30min, waits
After significantly increasing according to said ratio dimethoxy amino silane is added as coupling agent in its viscosity, control temperature at 100 DEG C persistently
Polyethers hydrophilic amino silicone oil is obtained after heating and thermal insulation 3h；
The synthesis of S3, polyether-containing aminopolysiloxane, equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
The polyethers hydrophilic amino silicone oil for preparing in S2 is added in four-hole boiling flask, isopropanol then is added according to said ratio, then plus
Heat heat preservation carries out back flow reaction between 80 DEG C, until reactant is transparent subsequent continuation of insurance temperature 3h, is finally evaporated under reduced pressure
It sloughs isopropanol and obtains polyether-containing aminopolysiloxane；
S4, high-performance flexible agent mixture, by organosilicon quaternary ammonium salt obtained above, polyethers hydrophilic amino silicone oil and
Polyethers hydrophilic amino silicone oil, which is added in mixing plant, uniformly to be mixed, and is according to the weight ratio organosilicon quaternary ammonium salt:
Polyethers hydrophilic amino silicone oil: then polyethers hydrophilic amino silicone oil 1:2:2 carries out high speed dispersion stirring until obtaining light yellow
The preparation of thick liquid completion high-performance flexible agent.
Embodiment two
A kind of high-performance flexible agent, including following component: chloropropyl triethoxysilane, octamethylcy-clotetrasiloxane, two
Methoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide, according to weight
Percentage is chloropropyl triethoxysilane 4%, octamethylcy-clotetrasiloxane 53%, dimethoxy amino silane 6%, active polyether
13%, tetramethylammonium hydroxide 0.2%, octadecyldimethyl ammonia 13%, isopropanol 13%, potassium iodide is a small amount of, chloropropyl three
The purity of Ethoxysilane is 98 percent.
The preparation of high-performance flexible agent includes the following steps:
The synthesis of S1, organosilicon quaternary ammonium salt, in four mouthfuls equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Octadecyldimethyl ammonia, isopropanol, chloropropyl triethoxysilane are sequentially added according to said ratio in flask, head is passed through nitrogen
Gas is stirred at low speed, and heating temperature is 83 DEG C, and in reflux temperature successive reaction 23h, then filtering solution removes insoluble anti-
Solvent and unreacted reactant are held in oxidant residue, finally vacuum distillation recycling, finally obtain in golden yellow organosilicon quaternary ammonium salt, finally
Micro dilution liquor kalii iodide is added as antioxidant, control pressure is in 0.02MPa；
The synthesis of S2, polyethers hydrophilic amino silicone oil are being equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Four-hole boiling flask according to said ratio be added octamethylcy-clotetrasiloxane, then carry out heating stir at low speed, control temperature exist
105 DEG C, tetramethylammonium hydroxide then is added as catalyst according to said ratio, then continuous heating keeps the temperature 35min, waits
After significantly increasing according to said ratio dimethoxy amino silane is added as coupling agent in its viscosity, control temperature at 105 DEG C persistently
Polyethers hydrophilic amino silicone oil is obtained after heating and thermal insulation 4h；
The synthesis of S3, polyether-containing aminopolysiloxane, equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
The polyethers hydrophilic amino silicone oil for preparing in S2 is added in four-hole boiling flask, isopropanol then is added according to said ratio, then plus
Heat heat preservation carries out back flow reaction between 83 DEG C, until reactant is transparent subsequent continuation of insurance temperature 3.3h, finally carries out decompression steaming
It evaporates and sloughs isopropanol and obtain polyether-containing aminopolysiloxane；
S4, high-performance flexible agent mixture, by organosilicon quaternary ammonium salt obtained above, polyethers hydrophilic amino silicone oil and
Polyethers hydrophilic amino silicone oil, which is added in mixing plant, uniformly to be mixed, and is according to the weight ratio organosilicon quaternary ammonium salt:
Polyethers hydrophilic amino silicone oil: then polyethers hydrophilic amino silicone oil 1:2:2 carries out high speed dispersion stirring until obtaining light yellow
The preparation of thick liquid completion high-performance flexible agent.
Embodiment three
A kind of high-performance flexible agent, including following component: chloropropyl triethoxysilane, octamethylcy-clotetrasiloxane, two
Methoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide, according to weight
Percentage is chloropropyl triethoxysilane 5%, octamethylcy-clotetrasiloxane 59%, dimethoxy amino silane 7%, active polyether
19%, tetramethylammonium hydroxide 0.3%, octadecyldimethyl ammonia 19%, isopropanol 14%, potassium iodide is a small amount of, chloropropyl three
The purity of Ethoxysilane is 98 percent.
The preparation of high-performance flexible agent includes the following steps:
The synthesis of S1, organosilicon quaternary ammonium salt, in four mouthfuls equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Octadecyldimethyl ammonia, isopropanol, chloropropyl triethoxysilane are sequentially added according to said ratio in flask, head is passed through nitrogen
Gas is stirred at low speed, and heating temperature is 89 DEG C, and in reflux temperature successive reaction 29h, then filtering solution removes insoluble anti-
Solvent and unreacted reactant are held in oxidant residue, finally vacuum distillation recycling, finally obtain in golden yellow organosilicon quaternary ammonium salt, finally
Micro dilution liquor kalii iodide is added as antioxidant, control pressure is in 0.03MPa；
The synthesis of S2, polyethers hydrophilic amino silicone oil are being equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Four-hole boiling flask according to said ratio be added octamethylcy-clotetrasiloxane, then carry out heating stir at low speed, control temperature exist
110 DEG C, tetramethylammonium hydroxide then is added as catalyst according to said ratio, then continuous heating keeps the temperature 40min, waits
After significantly increasing according to said ratio dimethoxy amino silane is added as coupling agent in its viscosity, control temperature at 110 DEG C persistently
Polyethers hydrophilic amino silicone oil is obtained after heating and thermal insulation 5h；
The synthesis of S3, polyether-containing aminopolysiloxane, equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
The polyethers hydrophilic amino silicone oil for preparing in S2 is added in four-hole boiling flask, isopropanol then is added according to said ratio, then plus
Heat heat preservation carries out back flow reaction between 89 DEG C, until reactant is transparent subsequent continuation of insurance temperature 3.6h, finally carries out decompression steaming
It evaporates and sloughs isopropanol and obtain polyether-containing aminopolysiloxane；
S4, high-performance flexible agent mixture, by organosilicon quaternary ammonium salt obtained above, polyethers hydrophilic amino silicone oil and
Polyethers hydrophilic amino silicone oil, which is added in mixing plant, uniformly to be mixed, and is according to the weight ratio organosilicon quaternary ammonium salt:
Polyethers hydrophilic amino silicone oil: then polyethers hydrophilic amino silicone oil 1:2:2 carries out high speed dispersion stirring until obtaining light yellow
The preparation of thick liquid completion high-performance flexible agent.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of high-performance flexible agent, which is characterized in that including following component: chloropropyl triethoxysilane, prestox ring four
Siloxanes, dimethoxy amino silane, active polyether, tetramethylammonium hydroxide, octadecyldimethyl ammonia, isopropanol, potassium iodide,
It is chloropropyl triethoxysilane 3-6%, octamethylcy-clotetrasiloxane 50-60%, dimethoxy amino silicone according to weight percent
Alkane 5-10%, active polyether 10-20%, tetramethylammonium hydroxide 0.1-0.5%, octadecyldimethyl ammonia 10-20%, isopropyl
Alcohol 12-15%, potassium iodide are a small amount of.
2. a kind of high-performance flexible agent according to claim 1, which is characterized in that the chloropropyl triethoxysilane
Purity is 98 percent.
3. a kind of high-performance flexible agent according to claim 1, which is characterized in that the preparation packet of the high-performance flexible agent
Include following steps:
The synthesis of S1, organosilicon quaternary ammonium salt, in the four-hole boiling flask that thermometer, blender, reflux condensing tube and nitrogen gas tank are housed
According to said ratio sequentially add octadecyldimethyl ammonia, isopropanol, chloropropyl triethoxysilane, head be passed through nitrogen into
Row stirs at low speed, and heating temperature is 80-90 DEG C, and in reflux temperature successive reaction 20-30h, then filtering solution is removed insoluble
Solvent and unreacted reactant are held in antioxidant residue, finally vacuum distillation recycling, finally obtain in golden yellow organosilicon quaternary ammonium salt；
The synthesis of S2, polyethers hydrophilic amino silicone oil, in four equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
Octamethylcy-clotetrasiloxane is added according to said ratio in mouth flask, then carries out heating and stirs at low speed, controls temperature in 100-
115 DEG C, tetramethylammonium hydroxide then is added as catalyst according to said ratio, then continuous heating keeps the temperature 30-45min,
Dimethoxy amino silane is added as coupling agent according to said ratio after waiting its viscosity to significantly increase, controls temperature in 100-
Polyethers hydrophilic amino silicone oil is obtained after 115 DEG C of continuous heating heat preservation 3-6h；
The synthesis of S3, polyether-containing aminopolysiloxane, in four mouthfuls equipped with thermometer, blender, reflux condensing tube and nitrogen gas tank
The polyethers hydrophilic amino silicone oil prepared in S2 is added in flask, isopropanol then is added according to said ratio, then heating is protected
Temperature carries out back flow reaction between 80-90 DEG C, until reactant is transparent subsequent continuation of insurance temperature 3-4h, is finally evaporated under reduced pressure
It sloughs isopropanol and obtains polyether-containing aminopolysiloxane；
S4, high-performance flexible agent mixture, by organosilicon quaternary ammonium salt obtained above, polyethers hydrophilic amino silicone oil and polyethers
Hydrophilic amino silicone oil is added in mixing plant and is uniformly mixed, and is according to the weight ratio organosilicon quaternary ammonium salt: polyethers
Hydrophilic amino silicone oil: then polyethers hydrophilic amino silicone oil 1:2:2 carries out high speed dispersion stirring until obtaining thick pale yellow
The preparation of liquid completion high-performance flexible agent.
4. a kind of high-performance flexible agent according to claim 1, which is characterized in that be additionally added in the step S1 micro
Liquor kalii iodide is diluted as antioxidant.
5. a kind of high-performance flexible agent according to claim 1, which is characterized in that be evaporated under reduced pressure in step S1, S3
When control pressure 0.01 between 0.04MPa.
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