CN109021237A - Big partial size organopolysiloxane elastomer lotion and its plastic toughening modifying agent being prepared - Google Patents
Big partial size organopolysiloxane elastomer lotion and its plastic toughening modifying agent being prepared Download PDFInfo
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- CN109021237A CN109021237A CN201810696706.4A CN201810696706A CN109021237A CN 109021237 A CN109021237 A CN 109021237A CN 201810696706 A CN201810696706 A CN 201810696706A CN 109021237 A CN109021237 A CN 109021237A
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- Prior art keywords
- partial size
- organopolysiloxane elastomer
- big partial
- lotion
- size organopolysiloxane
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 54
- 239000000806 elastomer Substances 0.000 title claims abstract description 51
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 51
- 239000006210 lotion Substances 0.000 title claims abstract description 36
- 229920003023 plastic Polymers 0.000 title claims abstract description 18
- 239000004033 plastic Substances 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 12
- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 150000001336 alkenes Chemical class 0.000 claims abstract description 8
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 125000000524 functional group Chemical group 0.000 claims description 22
- 239000000178 monomer Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 14
- 230000007062 hydrolysis Effects 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- -1 oxygen Alkane Chemical class 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 7
- 229920000126 latex Polymers 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000007792 addition Methods 0.000 description 8
- 238000009835 boiling Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000004816 latex Substances 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 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 4
- 238000006243 chemical reaction Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- 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
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
-
- 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
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a kind of big partial size organopolysiloxane elastomer lotion and its plastic toughening modifying agent being prepared, the particle size distribution range of the big partial size organopolysiloxane elastomer is 400~2300nm；The big partial size organopolysiloxane elastomer is cross-linked three D structure and have can reactive active group again；The big partial size organopolysiloxane elastomer lotion is obtained using emulsion polymerization technique.Big partial size organopolysiloxane elastomer lotion and unsaturated olefin described in the plastic toughening modifying agent use are obtained through emulsion polymerization.Big partial size organopolysiloxane elastomer of the invention, which not only has big partial size also, has wider particle size range, improve the dispersion performance and tinctorial property of rubber, after active group is added, applying above in the later period can polymerize with many high molecular materials, improve precipitation problem when later period modification high temperature process.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to organopolysiloxane elastomer reaction modifying field.
Background technique
Organic silicon rubber is because have the advantages that weatherability, high- and low-temperature resistance alternation and good flame resistance, and increasingly by people
Paid attention to, be will be used wider and wider.About the technology with organic siloxane modified other high molecular materials and using also layer
It is not poor out, but since organopolysiloxane elastomer is many kinds of and molecular structure is complicated, application field can very wide and specific aim pole
By force.And the dispersion performance of organopolysiloxane elastomer is poor, is easy the precipitation in high temperature process, and organopolysiloxane elastomer
Color is excessively poor.
The partial size of big partial size organopolysiloxane elastomer is wide, so as to allow tinctorial property to improve, but big partial size organosilicon oxygen
For the field of modified copolymer unsaturated olefin, but rarely people is related to alkane rubber.
Summary of the invention
The first technical problem to be solved by the present invention is: in view of the deficienciess of the prior art, providing a kind of big grain
Diameter organopolysiloxane elastomer lotion has the wider big partial size lotion of distribution, can be improved tinctorial property, and improve and divide
Dissipate performance.
Second technical problem to be solved by this invention is: in view of the deficienciess of the prior art, providing a kind of plastics
Plasticized modifier improves the low-temperature flexibility and flame retardant property of plastics for the toughening modifying of plastics.
In order to solve the first technical problem mentioned above, the technical scheme is that
Big partial size organopolysiloxane elastomer lotion, the particle size distribution range of the big partial size organopolysiloxane elastomer are 400
~2300nm；The big partial size organopolysiloxane elastomer is cross-linked three D structure and have can reactive active group again；Institute
Big partial size organopolysiloxane elastomer lotion is stated to obtain using emulsion polymerization technique.
As a kind of improved technical solution, the big partial size organopolysiloxane elastomer lotion is will be in organosilicon ring monomer
One or more, with containing there are three one of functional group or three or more organic silicon monomer of functional group or it is a kind of with
After upper mixing, acid is added in aqueous phase system or alkali carries out a kind of stable lotion of cohydrolysis acquisition.
As a kind of preferred technical solution, the organosilicon ring monomer include DMC (dimethicone mixture),
D4 (octamethylcyclotetrasiloxane), D5 (decamethylcyclopentaandoxane) and D6 (ten diformazan basic rings, six siloxanes).
It is described containing there are three the organic silicon monomers of functional group or three or more functional group as a kind of preferred technical solution
It is 4 organic silicon monomer of R-Si- (OR ') 3 or R-Si- (OR ')；The R ' is methyl or ethyl；The R is methyl, ethyl, third
Any one or more of base, glycidoxy, acryloxy, vinyl.
It is described containing there are three the organic of functional group or three or more functional group as a kind of further preferred technical solution
The preferred ethyl orthosilicate of silicon monomer and vinyl trimethylsilane；The ethyl orthosilicate and vinyl trimethylsilane weight ratio
Example is preferably 3~6:1~3.
As a kind of preferred technical solution, the organosilicon of the water and functional group or three or more functional group containing there are three
Monomer, organosilicon ring monomer weight ratio be 6~8:2~4.
It is described containing there are three the organic silicon monomers of functional group or three or more functional group as a kind of preferred technical solution
Mixed weight ratio with organosilicon ring monomer is 0.1~1.0:9.1~9.9.
It is described containing there are three the organic of functional group or three or more functional group as a kind of further preferred technical solution
The mixed weight ratio of silicon monomer and organosilicon ring monomer is 0.5~0.7:9.3~9.5.
As a kind of preferred technical solution, the hydrolysis temperature when hydrolysis is 20~85 DEG C.
As a kind of further preferred technical solution, the hydrolysis temperature when hydrolysis is 40~60 DEG C.
As a kind of preferred technical solution, the acid that when hydrolysis is added can be organic acid, be also possible to inorganic acid,
The pH value of water phase is adjusted between 2~4；The alkali of addition can be sodium hydroxide or potassium hydroxide, adjust the pH of water phase 11~
Between 12.
As a kind of further preferred technical solution, the organic acid that when hydrolysis is added is sulfonic acid, citric acid, propylene
Acid, maleic acid etc., inorganic acid are hydrochloric acid, sulfuric acid, phosphoric acid etc.；More preferable citric acid；The preferred potassium hydroxide of the alkali of addition.
To solve above-mentioned second technical problem, the technical scheme is that
A kind of plastic toughening modifying agent, big partial size organopolysiloxane elastomer cream described in the plastic toughening modifying agent use
Liquid and unsaturated olefin are obtained through emulsion polymerization.
As a kind of preferred technical solution, the weight ratio of big partial size organopolysiloxane elastomer and unsaturated olefin is 5~
85:15~95.
As a kind of further preferred technical solution, the weight ratio of big partial size organopolysiloxane elastomer and unsaturated olefin
For 5~50:50~95.
As a kind of preferred technical solution, the unsaturated olefin includes acrylate, styrene, acrylonitrile, Malaysia
One of acid esters, butadiene or more than one.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
Big partial size organopolysiloxane elastomer lotion of the invention, the particle diameter distribution model of the big partial size organopolysiloxane elastomer
It encloses for 400~2300nm；The big partial size organopolysiloxane elastomer is cross-linked three D structure and have can reactive activity again
Group；Not only there is big partial size also to have wider particle size range, improve the dispersion performance and tinctorial property of rubber, is added and lives
Property group after, in the later period, application above can polymerize with many high molecular materials, improve precipitation when later period modification high temperature process
Problem.
Plastics are obtained through emulsion polymerization using big partial size organopolysiloxane elastomer lotion and unsaturated olefin of the invention to increase
Tough modifying agent improves the low-temperature flexibility and flame retardant property of plastics for the toughening modifying of plastics.
Specific embodiment
Below with reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
Big partial size organopolysiloxane elastomer lotion, the big partial size organopolysiloxane elastomer lotion is by DMC, with positive silicic acid
After ethyl ester and vinyl trimethylsilane mixing, alkali (sodium hydroxide) pH value is added in aqueous phase system and is carried out jointly in 11-12
Hydrolyze the lotion that the particle size distribution range that (30 degree of hydrolysis temperature) obtains is 1800~2000nm.
Embodiment 2
Big partial size organopolysiloxane elastomer lotion, the big partial size organopolysiloxane elastomer lotion is by D4 (prestox four
Siloxanes), after being mixed with the ethyl orthosilicate and vinyl trimethylsilane that weight ratio is 3:2, it is added in aqueous phase system
Sour (hydrochloric acid) adjusts the pH value of water phase between 2~4, carries out the particle size distribution range that cohydrolysis (35 degree of hydrolysis temperature) obtains
For the lotion of 1600~1800nm.The water and D4 (octamethylcyclotetrasiloxane), ethyl orthosilicate and vinyl trimethylsilane
Weight ratio be 6:2.
Embodiment 3
Big partial size organopolysiloxane elastomer lotion, the big partial size organopolysiloxane elastomer lotion is by D6 (ten dimethyl
Six siloxanes of ring), after being mixed with the ethyl orthosilicate and vinyl trimethylsilane that weight ratio is 5:2, in aqueous phase system
The pH of alkali (sodium hydroxide) adjusting water phase is added 11~12, carries out the particle diameter distribution that cohydrolysis (32 degree of hydrolysis temperature) obtains
Range is the lotion of 2200~2300nm.The water and D6 (ten diformazan basic rings, six siloxanes), ethyl orthosilicate and vinyl three
The weight ratio of methyl-monosilane is 7:3.
Embodiment 4
(1) citric acid 6g is taken, it is good spare with 50 grams of deionized water dissolutions.
(2) DMC:93g, vinyl trimethylsilane 2g, ethyl orthosilicate 5g are spare after mixing.
(3) taking 350 grams of deionized waters to be added has in water bath with thermostatic control and four-hole boiling flask with agitating device, opens agitating device
To 100 revs/min, bath temperature is controlled at 55 DEG C constant speed.
(4) by 100 grams of DMC, vinyl trimethylsilane, ethyl orthosilicate mixed liquor addition four-hole boiling flasks, then between
50 grams of ready citric acid solution is added after 1 minute, bath temperature control hydrolyzes 20 hours at 55 degree DEG C and obtains big partial size
Organopolysiloxane elastomer samples of latex.
Embodiment 5
(1) potassium hydroxide 10g is taken, it is good spare with 50 grams of deionized water dissolutions.
(2) DMC95g, vinyl trimethylsilane 2g, ethyl orthosilicate 3g are spare after mixing.
(3) taking 350 grams of deionized waters to be added has in water bath with thermostatic control and four-hole boiling flask with agitating device, opens agitating device
To 100 revs/min, bath temperature is controlled at 50 DEG C constant speed.
(4) by 100 grams of DMC, vinyl trimethylsilane, ethyl orthosilicate mixed liquor addition four-hole boiling flasks, then between
50 grams of ready potassium hydroxide solution is added after 1 minute, bath temperature control hydrolyzes 20 hours at 50 DEG C and obtains big partial size
Organopolysiloxane elastomer samples of latex.
Embodiment 6
(1) hydrochloric acid 3g is taken, it is good spare with 50 grams of deionized water dissolutions.
(2) D4 (octamethylcyclotetrasiloxane) and D6 (ten diformazan basic rings, six siloxanes) 97g, vinyl trimethylsilane are taken
3g, ethyl orthosilicate 5g are spare after mixing.
(3) 350 grams of deionized water additions are taken to have in the four-hole boiling flask of water bath with thermostatic control, bath temperature is controlled at 60 DEG C.
(4) by D4 (octamethylcyclotetrasiloxane) and D6 (ten diformazan basic rings, six siloxanes), vinyl trimethylsilane, positive silicon
In 100 grams of addition four-hole boiling flasks of acetoacetic ester mixed liquor, 50 grams of ready hydrochloric acid solution, water-bath are added after being then spaced 1 minute
Temperature control hydrolyzes 20 hours at 60 DEG C and obtains big partial size organopolysiloxane elastomer samples of latex.
Embodiment 7
(1) sulfuric acid 3g is taken, it is good spare with 50 grams of deionized water dissolutions.
(2) D5 (decamethylcyclopentaandoxane) 96g is taken, vinyl trimethylsilane 3g, ethyl orthosilicate 3g are uniformly mixed
It is spare afterwards.
(3) 350 grams of deionized water additions are taken to have in the four-hole boiling flask of water bath with thermostatic control, bath temperature is controlled at 52 DEG C.
(4) by D5 (decamethylcyclopentaandoxane), vinyl trimethylsilane, 100 grams of ethyl orthosilicate mixed liquor additions
In four-hole boiling flask, 52 grams of ready sulfuric acid liquid is added after being then spaced 1 minute, bath temperature control is small in 45 DEG C of hydrolysis 20
When obtain big partial size organopolysiloxane elastomer samples of latex.
Embodiment 8
Each 500 grams of big partial size organopolysiloxane elastomer lotion that above-described embodiment 2,4,6,7 obtains are taken respectively, use hydroxide
Sodium adjusts pH to neutrality, then respectively with 2000 grams of deionized water, 500 grams of butyl acrylate, 5 grams of lauryl sodium sulfate, mistake
0.5 gram of potassium sulfate carries out the emulsion polymerization of hot initiation together, controls reaction temperature between 75~85 DEG C, obtains after the completion of polymerization
Silicon the third latex plastic toughening modifying agent sample 2-1,4-1,6-1,7-1 with high coloring performance, high-weatherability.
Embodiment 9
Each 500 grams of big partial size organopolysiloxane elastomer lotion that above-described embodiment 1,3,5 obtains are taken respectively, with citric acid tune
PH is saved to neutrality, then respectively with 2000 grams of deionized water, 500 grams of styrene, 5 grams of lauryl sodium sulfate, potassium peroxydisulfate 0.5
The emulsion polymerization of hot initiation gram is carried out together, controls reaction temperature between 75~85 DEG C, obtaining after the completion of polymerization has brilliant idea
Silicon the third latex plastic toughening modifying agent sample 1-1,3-1,5-1 of color performance, high-weatherability.
It can be used for PC, AS plastic toughening modifying after the plastic toughening modifying agent being prepared is dry, PC, AS can be allowed to mould
Material obtains extremely excellent low-temperature flexibility and anti-flammability.
The performance indicator for the plasticized modifier that above-described embodiment 8 and embodiment 9 are prepared is as shown in the table:
Claims (10)
1. big partial size organopolysiloxane elastomer lotion, it is characterised in that: the particle diameter distribution of the big partial size organopolysiloxane elastomer
Range is 400~2300nm；The big partial size organopolysiloxane elastomer be cross-linked three D structure and have can reactive work again
Property group；The big partial size organopolysiloxane elastomer lotion is obtained using emulsion polymerization technique.
2. big partial size organopolysiloxane elastomer lotion as described in claim 1, it is characterised in that: the big partial size organosilicon oxygen
Alkane rubber latex be by one of organosilicon ring monomer or more than one, and containing there are three functional group or three or more functional groups
One of organic silicon monomer or more than one mixing after, acid is added in aqueous phase system or alkali carries out cohydrolysis acquisition
A kind of stable lotion.
3. big partial size organopolysiloxane elastomer lotion as claimed in claim 2, it is characterised in that: the organosilicon ring monomer packet
Include DMC, D4, D5 and D6.
4. big partial size organopolysiloxane elastomer lotion as claimed in claim 2, it is characterised in that: described containing there are three functional groups
Or the organic silicon monomer of three or more functional groups is R-Si- (OR ')3Or R-Si- (OR ')4Organic silicon monomer；The R ' is methyl
Or ethyl；The R is any one or more of methyl, ethyl, propyl, glycidoxy, acryloxy, vinyl.
5. big partial size organopolysiloxane elastomer lotion as claimed in claim 4, it is characterised in that: described containing there are three functional groups
Or the preferred ethyl orthosilicate of organic silicon monomer and vinyl trimethylsilane of three or more functional groups.
6. partial size organopolysiloxane elastomer lotion as claimed in claim 2 big, it is characterised in that: when the hydrolysis water with contain
The organic silicon monomer of three functional groups or three or more functional group, the weight ratio of organosilicon ring monomer are 6~8:2~4.
7. big partial size organopolysiloxane elastomer lotion as claimed in claim 2, it is characterised in that: described containing there are three functional groups
Or the mixed weight ratio of the organic silicon monomer of three or more functional groups and organosilicon ring monomer is 0.1~1.0:9.1~9.9.
8. big partial size organopolysiloxane elastomer lotion as claimed in claim 2, it is characterised in that: the hydrolysis temperature when hydrolysis
Degree is 20~85 DEG C.
9. big partial size organopolysiloxane elastomer lotion as claimed in claim 2, it is characterised in that: the acid being added when the hydrolysis
It can be organic acid, be also possible to inorganic acid, adjust the pH value of water phase between 2~4；The alkali of addition can be sodium hydroxide or
Potassium hydroxide adjusts the pH value of water phase between 11~12.
10. a kind of plastic toughening modifying agent, it is characterised in that: the plastic toughening modifying agent uses as described in claim 1
Big partial size organopolysiloxane elastomer lotion and unsaturated olefin are obtained through emulsion polymerization.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114437300A (en) * | 2022-01-24 | 2022-05-06 | 青岛森特新材料科技有限公司 | Preparation method and application of halogen-free flame retardant toughening agent |
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| CN1329623A (en) * | 1998-12-04 | 2002-01-02 | 通用电气公司 | Emulsion polymerized silicone-acrylate rubber impact modifiers, thermoplastic blends, and methods for making |
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