CN109517191A - A kind of highly stable Modified silicon oil emulsion - Google Patents
A kind of highly stable Modified silicon oil emulsion Download PDFInfo
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- CN109517191A CN109517191A CN201811363577.3A CN201811363577A CN109517191A CN 109517191 A CN109517191 A CN 109517191A CN 201811363577 A CN201811363577 A CN 201811363577A CN 109517191 A CN109517191 A CN 109517191A
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- modified silicon
- silicon oil
- oil emulsion
- deionized water
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- 239000003921 oil Substances 0.000 title claims abstract description 70
- 239000000839 emulsion Substances 0.000 title claims abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- -1 polyoxyethylene Polymers 0.000 claims abstract description 61
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 42
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 12
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 12
- WQQPDTLGLVLNOH-UHFFFAOYSA-M sodium;4-hydroxy-4-oxo-3-sulfobutanoate Chemical compound [Na+].OC(=O)CC(C([O-])=O)S(O)(=O)=O WQQPDTLGLVLNOH-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 9
- 239000000194 fatty acid Substances 0.000 claims abstract description 9
- 229930195729 fatty acid Natural products 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 8
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical class C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229920002545 silicone oil Polymers 0.000 claims description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229940008099 dimethicone Drugs 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 3
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical group CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 3
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 2
- 229920002556 Polyethylene Glycol 300 Polymers 0.000 claims description 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 2
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims description 2
- LQNFHLFWAIRQSO-UHFFFAOYSA-N S(=O)(=O)(O)C(C(=O)OCCCCCC(C)C)CC(=O)OCCCCCC(C)C.S(=O)(=O)(O)C(C(=O)O)CC(=O)O Chemical compound S(=O)(=O)(O)C(C(=O)OCCCCCC(C)C)CC(=O)OCCCCCC(C)C.S(=O)(=O)(O)C(C(=O)O)CC(=O)O LQNFHLFWAIRQSO-UHFFFAOYSA-N 0.000 claims description 2
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 2
- YUCTUWYCFFUCOR-UHFFFAOYSA-N 1,4-dihexoxy-1,4-dioxobutane-2-sulfonic acid;sodium Chemical compound [Na].CCCCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCCCC YUCTUWYCFFUCOR-UHFFFAOYSA-N 0.000 claims 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 241000220324 Pyrus Species 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 235000021017 pears Nutrition 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 6
- 238000013112 stability test Methods 0.000 abstract description 3
- 238000000703 high-speed centrifugation Methods 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 54
- 150000003376 silicon Chemical class 0.000 description 27
- 229910052739 hydrogen Inorganic materials 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 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 description 5
- 239000000843 powder Substances 0.000 description 5
- HFDVRLIODXPAHB-UHFFFAOYSA-N 1-tetradecene Chemical compound CCCCCCCCCCCCC=C HFDVRLIODXPAHB-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 4
- 239000013067 intermediate product Substances 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000004816 latex Substances 0.000 description 3
- 229920000126 latex Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229940095068 tetradecene Drugs 0.000 description 2
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 description 1
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 208000005156 Dehydration Diseases 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229940102253 isopropanolamine Drugs 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3684—Treatment with organo-silicon compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2383/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—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
- C08J2483/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cosmetics (AREA)
Abstract
The present invention provides a kind of highly stable Modified silicon oil emulsion, the main components containing following parts by weight: 10-15 parts of dimethicones, 0.7-1.1 parts of long chain alkyl modified silicon oils, 0.5-1.2 parts of polyethylene glycol (PEG), 0.2-0.7 parts of polyoxyethylene aliphatic alcohol ethers, 0.5-1 parts of sorbitan fatty acid esters, 1-1.6 parts of alkyl phenol polyoxyethylene ether, 0.3-0.7 parts of sulfosuccinic acid sodium salt and 25-35 parts of deionized water.The Modified silicon oil emulsion high speed centrifugation, high temperature resistant, storage stability test in all show high stability, the dispersing agent as titanium white production has more wide applicability.Using Modified silicon oil emulsion of the present invention as titanium dioxide made from dispersing agent, good dispersion, especially oil-dispersing property are obviously improved.
Description
Technical field
The present invention relates to a kind of silicone oil emulsions, and in particular to it is a kind of for highly stable Modified silicon oil emulsion and its
Preparation method further relates to a kind of method for preparing titanium dioxide as dispersing agent using the Modified silicon oil emulsion.
Background technique
Titanium dioxide, main component are titanium dioxide, are had in industries such as coating, plastics, ink, papermaking, chemical fibre, ceramics wide
General application.Due to TiO2Specific grain surface product is big, specific surface energy with higher；Simultaneously titanium dioxide Ti-O bond distance it is small and
Length discrepancy, so that TiO2Molecular polarity is very strong, and the water of adsorption is dissociated because polarizing, and forms hydroxyl.In the life of titanium dioxide
In production and application process, due to TiO2Particle special physicochemical properties and surface characteristic, due to being not easy in apolar medium
Middle dispersion directly affects the performance of performance by being easy cohesion in polarizable medium.In the preparation, storage, use process of titanium dioxide
In, the degree of scatter of product, dispersion stabilization have very big shadow to the application performance of product, processing, use and final mass
It rings.
Currently, organic dispersing agent used in titanium white production, use process is mainly dimethyl silicone polymer, i.e. silicon
Oil.Silicone oil has excellent chemical stability, heat-resisting cold resistance, weatherability, lubricity, non-toxic to humans.Poly dimethyl
Siloxane main chain is a kind of spiral shape linear chain structure for easily disturbing song, and the energy required for the rotation of Si-O key is very low, therefore
Steric effect is unobvious when as dispersing agent, weak with titanium dioxide surface reaction forces, is easy in storage and use from titanium dioxide table
Emaciated face is fallen, and causes the storage stability and bad dispersibility of titanium dioxide.On the other hand, because of the hydrophobicity of dimethicone, in water
It is difficult to disperse in system, is restricted it in the application of aqueous medium, generally requires and be prepared as silicone oil emulsion.But due to silicone oil
Low surface tension and high viscosity, lead to more difficult emulsification, on the other hand, silicone oil itself is a kind of demulsifier, and lotion is made to be not easy to protect
It is fixed to keep steady.Therefore, preparing a kind of high stability silicone oil emulsion as divided titanium dioxide powder is still one that the field needs to solve
Hang-up.
Patent CN104559342A discloses a kind of divided titanium dioxide powder, contains isopropanolamine, N- isopropyl acrylamide
Amine, molecular weight are the silicone resin of 600-800, and molecular weight is the polyphosphazene polymer carbonic ester of 10000-11000, but its dispersing agent packet
Containing various ingredients, complicated component prepares complicated, and production cost is high, is not suitable for large-scale industrial production and application.
Patent CN108359277A discloses a kind of titanium white powder pigment dispersing agent, but the physics and chemistry without disclosing the dispersing agent
Property, dispersion performance and stability.
Patent CN107722676A discloses a kind of modified silicon oil as titanium dioxide organic process, wherein modified silicon oil
Side chain is referred in general formula can be grafted the C1-C12 alkyl replaced for C1-C2 alkoxysilyl group or carboxyl, but it is being implemented
Long alkyl is not prepared in example and is the modified silicon oil of side chain, and does not refer to the stability of modified silicon oil.And
Its non-self-control of modified silicon oil used, but it is directly purchased from market, it can not be conveniently adjusted the length and quantity of side chain, also with regard to nothing
Method obtains the Modified silicon oil emulsion of different performance to meet the actual demand of titanium white production.
Summary of the invention
To solve the above problems, the purpose of the present invention is to provide a kind of highly stable Modified silicon oil emulsion, conduct
Divided titanium dioxide powder dispersion effect is good and dispersion stabilization is strong.
The present invention is realized by following technical proposals:
A kind of Modified silicon oil emulsion, the main component containing following parts by weight: 10-15 parts of dimethicones, 0.7-1.1 parts
Long chain alkyl modified silicon oil, 0.5-1.2 part polyethylene glycol (PEG), 0.2-0.7 parts of polyoxyethylene aliphatic alcohol ethers, 0.5-1 parts of dehydrations
Span, 1-1.6 part alkyl phenol polyoxyethylene ether, 0.3-0.7 parts of sulfosuccinic acid sodium salt and 25-35 parts are gone
Ionized water.
Preferably, long chain alkyl modified silicon oil has the structure of formula (1),
Wherein R is the alkyl that carbon atom number is 12-18, preferably dodecyl, myristyl, cetyl；M:n is
0.25-0.4:1。
In an optimal technical scheme of the invention, the silicone oil emulsion, the main component containing following parts by weight:
12-14 parts of dimethicones, 0.5-0.8 parts of long chain alkyl modified silicon oils, 0.7-0.9 parts of polyethylene glycol (PEG), 0.25-0.4 parts
Polyoxyethylene aliphatic alcohol ether, 0.7-0.85 part sorbitan fatty acid ester, 1.2-1.4 parts of alkyl phenol polyoxyethylene ether, 0.35-
The deionized water of 0.5 part of sulfosuccinic acid sodium salt and 28-33 part.
Preferably, the polyethylene glycol is selected from at least one of PEG200, PEG300, PEG400, PEG500, PEG600.
Preferably, the polyoxyethylene aliphatic alcohol ether is selected from AEO-3, AEO-4 and AEO-5.
Preferably, the sorbitan fatty acid ester is selected from Span40, Span60 and Span80.
Preferably, the alkyl phenol polyoxyethylene ether is selected from OP-10, SOPE-10, TX10 and TX12.
Preferably, the sulfosuccinic acid sodium salt is selected from two cyclohexyl ester sodium salt (B-196) of sulfosuccinic acid, sulfosuccinic acid
Dihexyl sodium salt (B-8084) and sulfosuccinic acid diisooctyl sulfosuccinate (OT-75).
The present invention also provides a kind of preparation methods of Modified silicon oil emulsion, comprising the following steps:
(1), according to formula by emulsifier polyoxyethylene fatty alcohol ether, sorbitan fatty acid ester, alkyl phenol polyoxy second
Alkene ether and sulfosuccinic acid sodium salt are added to dry anhydrous reaction kettle, stir evenly；
(2), dimethicone and long alkane under agitation, are added into the good emulsifier mixture of above-mentioned compounding
Base modified silicon oil, and slurry in kettle is kept to be again stirring for uniformly, deionized water being slowly added to, when mixture viscosity at 60-90 DEG C
Reach maximum, stop stirring and add water, scrapes wall；
(3) by after paste scrapes reaction kettle on wall, continue to stir, remaining deionized water is faster added, continues to stir
It is cooled to room temperature after 1-3 hours, by reaction solution by collecting product after homogenizer homogeneous.
When deionized water is added in above-mentioned steps, deionized water temperature is consistent with slurry temperature in reaction kettle.
The present invention also provides a kind of method for preparing titanium dioxide, specifically: by titanium dioxide deionized water stirring to pulp,
The slurry that concentration is 240-260g/L concentration is obtained, Modified silicon oil emulsion of the present invention is added thereto, stirs 30min
Afterwards, 110 DEG C of dry 12h carry out airslide disintegrating mill crushing, obtain titanium dioxide after grinding.
Compared to the prior art, Modified silicon oil emulsion provided by the invention has the following characteristics that
One, it is compounded using long chain alkyl modified silicon oil and dimethicone, the Modified silicon oil emulsion of high stability is made, led to
It crosses and silicone oil is modified with chain alkyl, realize the modified silicon oil property excellent as dispersing agent in titanium white production
Energy；
Two, specific nonionic emulsifier and anionic emulsifier compounding are selected, two kinds of emulsifier alternating sorbents exist
Emulsion particle surface forms compound emulsifying agent interface, and preferably suitable proportion realizes Modified silicon oil emulsion height obtained
Stablize, production application needs are able to satisfy in every stability test.
Three, using Modified silicon oil emulsion of the present invention as titanium dioxide made from dispersing agent, good dispersion, especially oil dispersed
Property is obviously improved.
Four, the present invention also provides a kind of methods, can be by adjusting long alkyl side chain in long chain alkyl modified silicon oil
Length and quantity, are prepared the modified silicon oil of different cultivars, and then prepare a variety of different in moisture with can be convenient dissipate property/oil
The titanium dioxide for dissipating property, meets different industrial application demands.
Specific embodiment:
In order to be further understood that summary of the invention of the invention, the present invention is elaborated below in conjunction with specific embodiment.
Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
The portion of reagent source that the present invention uses is as described below:
Dimethicone (201), high containing hydrogen silicone oil (202), purchased from Jiangxi letter along Chemical Co., Ltd.；
Octamethylcy-clotetrasiloxane (D4) is purchased from Shandong West Asia chemical industry Co., Ltd；
Hexamethyldisiloxane (MM) is purchased from Jiangxi the lucky star Chemical Co., Ltd.；
1- dodecylene, tetradecene, cetene are purchased from Jin Jinle Chemical Co., Ltd.；
Polyoxyethylene aliphatic alcohol ether (AEO-3, AEO-4, AEO-5) is purchased from Zou Yang Chemical Co., Ltd.；
Water Span (Span40, Span60, Span80), alkyl phenol polyoxyethylene ether (OP-10, TX10,
TX12) it is purchased from Hubei Xin Runde Chemical Co., Ltd.；
Sulfosuccinic acid sodium salt (B-196, B-8084, OT-75) is purchased from Shanghai loyalty Fine Chemical Co., Ltd.
The preparation of long chain alkyl modified silicon oil:
The method that the preparation method of the long chain alkyl modified silicon oil is referred to CN101434702A record.Specially
By high containing hydrogen silicone oil (202), the octamethylcy-clotetrasiloxane (D centainly matched4) and hexamethyldisiloxane (MM) reaction, it is added
5% concentrated sulfuric acid of the above material gross mass is catalyst, is reacted 3-6 hours under the conditions of 60-70 DEG C, at 120-140 DEG C,
Volatile materials is steamed under 0.1MPa vacuum condition, obtains silicon oil of low hydrogen content (PHMS) intermediate product.Under nitrogen protection state,
Catalyst H is added into the alpha-olefin that carbon chain lengths are 12-182PtCl6, above-mentioned silicon oil of low hydrogen content is added to the mode of dropwise addition
(PHMS) it in, is reacted 1-4 hours under the conditions of 80 DEG C；Volatile materials is steamed under 120-140 DEG C, O.OlMPa pressure, is obtained
Long chain alkyl modified silicon oil.
The present invention has obtained the modified silicon oil of the alkyl side chain of different carbon atoms according to above-mentioned preparation method.Specific steps are such as
Under:
(1), the preparation of silicon oil of low hydrogen content (PHMS) intermediate product: silicon oil of low hydrogen content (PHMS): by high containing hydrogen silicone oil
(202), octamethylcy-clotetrasiloxane (D4) and hexamethyldisiloxane (MM) be added to reaction kettle according to a certain ratio, be added with
5% concentrated sulfuric acid of upper material gross mass is catalyst, is reacted 3-6 hours under the conditions of 60-70 DEG C, at 120-140 DEG C, 0.1MPa
Volatile materials is steamed under vacuum condition, obtains silicon oil of low hydrogen content (PHMS) intermediate product.By adjusting high containing hydrogen silicone oil
(202), octamethylcy-clotetrasiloxane (D4) proportion obtain m:n ratio different in formula (1) structure, the ratio of m and n can be by
It is roughly calculated to obtain according to following formula,
M (202) is the quality of high containing hydrogen silicone oil (202), m (D4) it is prestox ring
Tetrasiloxane (D4) quality.The dosage of hexamethyldisiloxane (MM) is high containing hydrogen silicone oil (202), octamethylcy-clotetrasiloxane
(D4) 2-4wt%.
(2), the preparation of long alkyl chain modified silicon oil: under nitrogen protection state, the α-alkene for being 12-16 to carbon chain lengths
Catalyst H is added in hydrocarbon2PtCl6, alpha-olefin (1- dodecylene, tetradecene, cetene) is added drop-wise to above-mentioned low contain
In hydrogen silicone oil (PHMS) intermediate product.It is reacted 1-4 hours under the conditions of 80 DEG C；It is steamed under 120-140 DEG C, O.OlMPa pressure
Volatile materials obtains long chain alkyl modified silicon oil.The proportion of PHMS and alpha-olefin according to Si-H:C=C molar ratio 1:1 ratio,
The quantity of Si-H can be calculated by the reactive hydrogen mass fraction of high containing hydrogen silicone oil (202), high Silicon Containing Hydrogen used in the present invention
Oily (202) reactive hydrogen mass fraction is 1.567%.
The sample number into spectrum of gained long alkyl chain modified silicon oil, raw material, composition and property are as shown in table 1.
Table 1
The configuration of silicone oil emulsion: (embodiment 1-12 and comparative example 1-3)
Silicone oil emulsion configures obtain as steps described below:
(1), according to formula by emulsifier polyoxyethylene fatty alcohol ether, sorbitan fatty acid ester, alkyl phenol polyoxy second
Alkene ether and sulfosuccinic acid sodium salt are added to dry anhydrous reaction kettle, stir evenly；
(2), dimethicone and long alkane under agitation, are added into the good emulsifier mixture of above-mentioned compounding
Base modified silicon oil, and slurry in kettle is kept to be again stirring for uniformly, deionized water being slowly added to, when mixture viscosity at 60-90 DEG C
Reach maximum, stop stirring and add water, scrapes wall；
(3) by after paste scrapes reaction kettle on wall, continue to stir, remaining deionized water is faster added, continues to stir
It is cooled to room temperature after 1-3 hours, by reaction solution by collecting product after homogenizer homogeneous.
When deionized water is added in above-mentioned steps, deionized water temperature is consistent with slurry temperature in reaction kettle.
It configures the component for obtaining silicone oil emulsion and proportion is listed in table 2, all components in parts by weight, obtain embodiment 1-
12 silicone oil emulsion.
Table 2
Comparative example 1-3
Influence for test long chain alkyl modified silicon oil to silicone oil emulsion performance, has prepared the silicone oil emulsion of comparative example 1-3.
Comparative example 1, other steps are identical as the embodiment of the present invention 3, only without addition long chain alkyl modified silicon oil.
Comparative example 2, other steps are identical as the embodiment of the present invention 5, only without addition long chain alkyl modified silicon oil.
Comparative example 3, other steps are identical as the embodiment of the present invention 7, only without addition long chain alkyl modified silicon oil.
The analysis of Modified silicon oil emulsion measures:
Following test is carried out to the silicone oil emulsion of above-described embodiment 1-12 and comparative example 1-3, as a result as described in Table 4.
Viscosimetric analysis:
Rotor is rotated 1-3min by rotational viscometer method in test solution, after stable reading, is read.Maintain sample
It is temperature-resistant, repetitive operation, using the arithmetic average of METHOD FOR CONTINUOUS DETERMINATION result three times as sample viscosity.
Determination of solid content:
Certain mass silicone oil emulsion sample is weighed with weighing bottle, is placed in 110 DEG C of constant temperature convection ovens and stands 3-5 hours extremely
Constant weight calculates solid content according to the following formula.
Quality × 100% before quality/sample dries after quality-sample dries before solid content=sample dries
Stability test:
1. centrifugal stability: samples of latex being added in centrifuge tube, is put into supercentrifuge, with 3000r/min speed
It is centrifuged 30min, lotion then shows emulsion-stabilizing without layering, floating oil, demulsifying phenomenon.
2. heat-resistant stability: taking appropriate samples of latex in weighing bottle, cover, static 24 hours in 60 DEG C of baking ovens
Afterwards, lotion then shows emulsion-stabilizing without layering, floating oil, demulsifying phenomenon.
3. storage stability: taking appropriate samples of latex, stored 6 months at 25 DEG C, lotion is existing without layering, floating oil, demulsification
As then showing emulsion-stabilizing.
The opinion rating of stability is as shown in table 3, not fuel-displaced, and stability scoring is 10, water outlet, and stability scoring is 0.
Table 3
Table 4
It can be seen that Modified silicon oil emulsion provided by the invention in high speed centrifugation, 60 DEG C of height by the correlation data of table 4
The stability that height is all had under conditions of temperature and at room temperature storage half a year, illustrates the addition of long chain alkyl modified silicon oil simultaneously
The stability of silicone oil emulsion is not adversely affected.Modified silicon oil emulsion provided by the invention as titanium white production,
As dispersing agent in using, different processing, use condition can satisfy, the adaptability with height,
The preparation and performance test of titanium dioxide:
1, Testing index and method
The detection method of water dispersible:
It takes the titanium dioxide sample to be measured of 15.00g in 100mL graduated cylinder, water is added and is beaten and adjusts volume to 100mL, in
The drying of 2mL solution is drawn with syringe at 80mL scale and claims to obtain residue weight m1, is stood 5 and is as a child sampled 2mL at 80mL
Residue is dried to obtain, the ratio of quality m2, m2 and m1 are the water dispersible index value of titanium dioxide sample.
The detection method of oil-dispersing property (the graceful value of black square): it is measured by Hegman grind gage, specifically according to patent
The method detection that CN104194409A is recorded.
Whiteness: the titanium dioxide after weighing 3g coating is uniformly mixed with the linseed oil of 1g, thick by after mixing
Titanium dioxide be uniformly coated on glass slide, be that 100 μm of wet film makers produce 100 μm of paint film, room temperature decentralization with specification
It is dry to coating, CIE color difference is measured with whiteness instrument.
2, the preparation of titanium white part
Using above-described embodiment 3,5,7 and the silicone oil emulsion of comparative example 1 as application of dispersant in the system of titanium dioxide
Method that is standby, being recorded in preparation step referenced patent CN106221297A and CN107722676A, specific as follows:
Embodiment 13
200g NR950 rutile type titanium white (purchased from golden Pu titanium industry) is taken, with deionized water stirring to pulp, obtains concentration
For the slurry of 240-260g/L concentration, silicone oil emulsion made from the 0.72g embodiment of the present invention 3 is added thereto, stirs 30min
Afterwards, 110 DEG C of dry 12h.Airslide disintegrating mill crushing is carried out after grinding, obtains titanium dioxide sample.
Embodiment 14
Use silicone oil emulsion made from the 0.72g embodiment of the present invention 5 as dispersing agent, other steps and 13 phase of embodiment
Together.
Embodiment 15
Use silicone oil emulsion made from the 0.72g embodiment of the present invention 7 as dispersing agent, other steps and 13 phase of embodiment
Together.
Comparative example 4
Use silicone oil emulsion made from 0.74g comparative example 1 of the present invention as dispersing agent, other steps and 13 phase of embodiment
Together.
3, testing result
Embodiment 13-15 and 4 gained titanium dioxide sample of comparative example are tested, the results are shown in Table 5.
Table 5
By the correlation data of table 5 it is found that the titanium white that Modified silicon oil emulsion provided by the invention is prepared as dispersing agent
Powder dispersibility is excellent, and especially in the case where influencing less on other performances, titanium dioxide sample oil-dispersing property is obviously improved.According to
This, the present invention provides a kind of methods, can be convenient by the length and quantity of long alkyl side chain in adjusting Modified silicon oil emulsion
Ground prepares the titanium dioxide that various different in moisture dissipate property/oil-dispersing property, meets different industrial application demands.Raw material of the present invention is easy
, method is simple, and the uniform and stable property of product property is good, there is good application prospect.
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 (8)
1. a kind of Modified silicon oil emulsion, the main component containing following parts by weight: 10-15 parts of dimethicones, 0.7-1.1 parts long
Alkyl group modified silicon oil, 0.5-1.2 part polyethylene glycol (PEG), 0.2-0.7 parts of polyoxyethylene aliphatic alcohol ethers, 0.5-1 parts of dehydration mountains
Pears alcohol fatty acid ester, 1-1.6 part alkyl phenol polyoxyethylene ether, 0.3-0.7 parts of sulfosuccinic acid sodium salt and 25-35 parts go from
Sub- water.
2. Modified silicon oil emulsion according to claim 1, which is characterized in that the main component containing following parts by weight: 12-
14 parts of dimethicones, 0.5-0.8 parts of long chain alkyl modified silicon oils, 0.7-0.9 parts of polyethylene glycol (PEG), 0.25-0.4 parts it is poly-
Ethylene oxide fatty alcohol ether, 0.7-0.85 part sorbitan fatty acid ester, 1.2-1.4 parts of alkyl phenol polyoxyethylene ether, 0.35-
The deionized water of 0.5 part of sulfosuccinic acid sodium salt and 28-33 part.
3. Modified silicon oil emulsion according to claim 1, which is characterized in that the long chain alkyl modified silicon oil has formula
(1) chemical formula,
Wherein R is the alkyl that carbon atom number is 12-18, preferably dodecyl, myristyl, cetyl.
4. Modified silicon oil emulsion according to claim 3, which is characterized in that in chemical formula shown in the formula (1), m:n is
0.25-0.4:1。
5. Modified silicon oil emulsion according to claim 1-4, which is characterized in that the polyethylene glycol is selected from
At least one of PEG200, PEG300, PEG400, PEG500, PEG600；The polyoxyethylene aliphatic alcohol ether be selected from AEO-3,
AEO-4 and AEO-5；The sorbitan fatty acid ester is selected from Span40, Span60 and Span80；The alkyl phenol polyoxy second
Alkene ether is selected from OP-10, SOPE-10, TX10 and TX12；The sulfosuccinic acid sodium salt is selected from two cyclohexyl ester sodium salt of sulfosuccinic acid
(B-196), sodium bishexyl sulfosuccinate (B-8084) and sulfosuccinic acid diisooctyl sulfosuccinate (OT-75).
6. the preparation method of Modified silicon oil emulsion according to claim 1, which comprises the following steps:
(1), according to formula by emulsifier polyoxyethylene fatty alcohol ether, sorbitan fatty acid ester, alkyl phenol polyoxyethylene ether
It is added to dry anhydrous reaction kettle with sulfosuccinic acid sodium salt, is stirred evenly；
(2), dimethicone under agitation, is added into the good emulsifier mixture of above-mentioned compounding and chain alkyl changes
Property silicone oil, and keep in kettle slurry at 60-90 DEG C, be again stirring for uniformly, deionized water being slowly added to, when mixture viscosity reaches
Maximum stops stirring and adds water, scrapes wall；
(3) by after paste scrapes reaction kettle on wall, continue to stir, remaining deionized water is faster added, continue to stir 1-3
It is cooled to room temperature after hour, by reaction solution by collecting product after homogenizer homogeneous；
When deionized water is added in above-mentioned steps, deionized water temperature is consistent with slurry temperature in reaction kettle.
7. the purposes of Modified silicon oil emulsion according to claim 1, which is characterized in that the dispersion as titanium white production
Agent.
8. a kind of method for preparing polymolecularity titanium dioxide, comprising the following steps: by titanium dioxide deionized water stirring to pulp, obtain
It is the slurry of 240-260g/L concentration to concentration, Modified silicon oil emulsion described in claim 1 is added thereto as dispersing agent,
After stirring 30min, 110 DEG C of dry 12h carry out airslide disintegrating mill crushing, obtain polymolecularity titanium dioxide after grinding.
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