CN109867808A - A kind of high rebound foam organic silicon surfactant and preparation method - Google Patents
A kind of high rebound foam organic silicon surfactant and preparation method Download PDFInfo
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- 239000006260 foam Substances 0.000 title claims abstract description 46
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 37
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract description 37
- 229920002545 silicone oil Polymers 0.000 claims abstract description 37
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 24
- 229920000570 polyether Polymers 0.000 claims abstract description 24
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 12
- 229920002635 polyurethane Polymers 0.000 claims abstract description 10
- 239000004814 polyurethane Substances 0.000 claims abstract description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 74
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 18
- 230000000694 effects Effects 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000003426 co-catalyst Substances 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003377 acid catalyst Substances 0.000 claims description 12
- 229920005862 polyol Polymers 0.000 claims description 12
- 150000003077 polyols Chemical class 0.000 claims description 12
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 10
- 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 description 10
- 230000002378 acidificating effect Effects 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 229940043237 diethanolamine Drugs 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- LJDSTRZHPWMDPG-UHFFFAOYSA-N 2-(butylamino)ethanol Chemical compound CCCCNCCO LJDSTRZHPWMDPG-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims 2
- 125000004432 carbon atom Chemical group C* 0.000 claims 2
- 229940058015 1,3-butylene glycol Drugs 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 230000003213 activating effect Effects 0.000 claims 1
- 235000019437 butane-1,3-diol Nutrition 0.000 claims 1
- DIVDFFZHCJEHGG-UHFFFAOYSA-N oxidopamine Chemical compound NCCC1=CC(O)=C(O)C=C1O DIVDFFZHCJEHGG-UHFFFAOYSA-N 0.000 claims 1
- 229920005830 Polyurethane Foam Polymers 0.000 abstract description 14
- 239000011496 polyurethane foam Substances 0.000 abstract description 14
- 238000010008 shearing Methods 0.000 abstract description 4
- 238000009423 ventilation Methods 0.000 abstract description 4
- 238000013461 design Methods 0.000 abstract description 2
- 206010000269 abscess Diseases 0.000 description 11
- 229910007161 Si(CH3)3 Inorganic materials 0.000 description 8
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 8
- 229920005573 silicon-containing polymer Polymers 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000005864 Sulphur Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000003999 initiator Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- -1 poly- methyl silicon Oxygen alkane Chemical class 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- AXPZIVKEZRHGAS-UHFFFAOYSA-N 3-benzyl-5-[(2-nitrophenoxy)methyl]oxolan-2-one Chemical compound [O-][N+](=O)C1=CC=CC=C1OCC1OC(=O)C(CC=2C=CC=CC=2)C1 AXPZIVKEZRHGAS-UHFFFAOYSA-N 0.000 description 1
- NRTLIYOWLVMQBO-UHFFFAOYSA-N 5-chloro-1,3-dimethyl-N-(1,1,3-trimethyl-1,3-dihydro-2-benzofuran-4-yl)pyrazole-4-carboxamide Chemical compound C=12C(C)OC(C)(C)C2=CC=CC=1NC(=O)C=1C(C)=NN(C)C=1Cl NRTLIYOWLVMQBO-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940031098 ethanolamine Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of high rebound foam organic silicon surfactant and preparation methods, belong to technical field of surfactant, solve the problems, such as polyurethane high resilience foam Miscibility in the prior art and polyurethane foam surface and dimensional stability.The containing hydrogen silicone oil that the present invention passes through two kinds of different structures of design, the allyl polyether different from molecular weight reacts to obtain the organic silicon modified by polyether surfactant of two kinds of different structures, regulate and control the ratio of different component, to realize the opening of polyurethane high resilience foam body and the balance of stability, to meeting high resilience polyurethane foam to the particular/special requirement of volume, ventilation, shearing, surface and dimensional stability, the problem of effective solution surface and the dimensional stability of Miscibility and polyurethane foam.
Description
Technical field
The present invention relates to a kind of surfactants and preparation method thereof, more particularly to a kind of high rebound foam organosilicon
Surfactant and preparation method, belong to technical field of surfactant.
Background technique
High resilience polyurethane foam (HR) is the foamed plastics of a kind of function admirable, and development is rapid at present,
It is widely used.The product is characterized in: have the characteristics that it is light, spring back, sound-absorbing damping, while also with the hand as latex
Sense, initial feel soft comfortable when further compression, and can provide solid and limber support, be a kind of ideal
Paving, cushion material, therefore it is largely used to seat, the back cushion, headrest of the production vehicles (automobile, train, aircraft etc.).
In high-rebound polyurethane foaming process, surfactant play the role of it is very important, to the abscess of foam
Mobility, foam smell when the adjustment of structure, foaming etc. have more apparent effect, especially in the knot for adjusting abscess
Structure and percent opening, while improving the compatibility of system.
In order to meet and widen all kinds of property need of the organic silicon surfactant in terms of high resilience polyurethane foam
It asks, it is increasing as the research of the modified silicon oil of raw material using containing hydrogen silicone oil, currently used for preparing high resilience polyurethane foam body
Silicone surfactant is generally dimethyl silicone polymer, organic functional dimethyl silicone polymer or polyether silicon copolymerization
Object.
Chinese patent CN105860084 reports a kind of organic silicon surfactant of low volatility, by containing hydrogen silicone oil with
At least one allyl ethyl polyethylene-oxide ether is prepared by hydrosilylation.By designing the structure of containing hydrogen silicone oil, alkene
The structure of propyl polyethylene glycol oxide ether realizes the opening of polyurethane moulding high rebound foam body and the balance of stability jointly;
Chinese patent CN1294141 report it is a kind of for producing the silicone surfactant of open-cell polyurethane flexible foam, should
Surfactant main component is dimethyl silicone polymer composition containing, and wherein dimethyl silicone polymer molecule content is at least
90%;United States Patent (USP) US4347330 is disclosed using including a kind of polysiloxane-polyoxyalkylene copolymer, a kind of poly- methyl silicon
Oxygen alkane and a kind of three kinds of pore regulators of the polyether polyhydroxy-compound pore regulator containing polyoxyethylene group prepare high rebound
The aperture flexible polyurethane foam of power;United States Patent (USP) US4139503 disclose using special silicone components prepare it is high-elastic
Property, aperture polyurethane foam, wherein using polyether polyol as solvent, active component siloxanes ratio is 0.01-2%, should
Patent only lists the embodiment of dimethyl silicone polymer.
Above-mentioned report mostly using dimethyl silicone polymer as cell opener, due to dimethyl silicone polymer hydrophobicity compared with
By force, poor with Miscibility, the surfactant that especially Chinese patent CN1294141 is reported is with dimethyl silicone polymer
Main component, and chain number n is 5-7, more demanding for component structure, controllable range is relatively narrow, limits its scope of application.
Simultaneously with high rebound foam in different products multiple demands, single organic silicon modified by polyether surfactant is
It is not able to satisfy high resilience polyurethane foam to the particular/special requirement of volume, ventilation, shearing, surface and dimensional stability.
Summary of the invention
The main object of the present invention is to solve polyurethane high resilience foam Miscibility and polyurethane foam in the prior art
The problem of foam body surface face and dimensional stability, and a kind of high rebound foam organic silicon surfactant preparation method is provided.
The purpose of the present invention can reach by using following technical solution:
A kind of high rebound foam organic silicon surfactant foams for polyurethane high resilience foam, the surface-active
Agent is grouped as by tri- kinds of groups of A, B, C, wherein shown in the structural formula of component A following (1):
In structural formula (1): the value that the value of m is 2~15, n is 1~10, and the value of m+n is 3~15;
The structure of R are as follows:-CH2CH2CH2O(CH2CH2O)a(CH2CH(CH3)O)bR1, the value that wherein value of a is 1~7, b is 0
The value of~7, a+b are the alkyl that 1~10, R1 is 1~4 carbon atom number;
Wherein, shown in the structural formula following (2) of B component:
In structural formula (2): the value that the value of m is 1~25, n is 1~15, and the value of m+n is 2~25;
The structure of R are as follows:-CH2CH2CH2O(CH2CH2O)a(CH2CH(CH3)O)bR2, the value that the value of a is 0~20, b is 1~
20, a+b value is the alkyl that 1~20, R2 is 1~4 carbon atom number;
Wherein, component C is the copolymer with the terminal hydroxyl as derived from polyol.
The usage percentage of component A is 20-40%, and the usage percentage of B component is 20-40%, the dosage percentage of component C
Than for 20-60%.
Component C is the copolymer with the terminal hydroxyl as derived from polyol, and polyol is low molecule
Weight polyalcohol, including ethylene glycol, propylene glycol, 1,3-BDO, 1,4-butanediol, 1,6- hexylene glycol, neopentyl glycol, diethylene glycol (DEG) and
Dipropylene glycol.
A kind of preparation method of high rebound foam organic silicon surfactant, includes the following steps:
Step 1: containing hydrogen silicone oil preparation
Using octamethylcy-clotetrasiloxane, high containing hydrogen silicone oil and hexamethyldisiloxane as raw material, in acidic catalyst effect
Under, under the conditions of reaction temperature is 30~90 DEG C, 5~8h is reacted, the containing hydrogen silicone oil of different structure is obtained;
Step 2: the preparation of component A and component B
Allyl polyether, chloroplatinic acid catalyst, the co-catalysis of above-mentioned resulting at least one containing hydrogen silicone oil and different structure
Agent is added in reactor, and normal pressure is warming up to 90-160 DEG C, reacts 2~8h, obtains two kinds of organic silicon modified by polyether surfactants:
Component A and B;
Step 3: the preparation of high rebound foam organic silicon surfactant
Resulting component A and B and component C are mixed according to different weight ratio, obtain high rebound foam with organic
Silicon surface active agent.
In step 1, acidic catalyst is at least one of Emathlite, sulfuric acid, trifluoromethanesulfonic acid and acidic resins.
Acidic catalyst is sulfuric acid, and dosage is the 1~2% of quality of material used.
In step 2, chloroplatinic acid catalyst is platinum catalyst, and platinum dosage is the 3-20ppm of material total amount.
In step 2, co-catalyst be diethanol amine, triethanolamine, acetamide, triethylamine and N- butylethanolamine in extremely
Few one kind.
Co-catalyst dosage is 3~80ppm of material total amount.
In step 3, the weight percent of component A is 20-40%, and the weight percent of component B is 20-40%, component C's
Weight percent is 20-60%.
Advantageous effects of the invention:
A kind of high rebound foam organic silicon surfactant preparation method provided by the invention, by designing two kinds not
Isostructural containing hydrogen silicone oil, the allyl polyether different from molecular weight react to obtain the organic silicon modified by polyether of two kinds of different structures
Surfactant regulates and controls the ratio of different component, the opening of Lai Shixian polyurethane high resilience foam body and the balance of stability,
To meet high resilience polyurethane foam to the particular/special requirement of volume, ventilation, shearing, surface and dimensional stability, effective solution
The problem of surface and dimensional stability of Miscibility and the polyurethane foam of having determined.
Specific embodiment
To make the more clear and clear technical solution of the present invention of those skilled in the art, the present invention is made below further
Detailed description, embodiments of the present invention are not limited thereto.
Embodiment 1:
(1) component A1Synthesis
By 94.93g octamethylcy-clotetrasiloxane, 51.71g high containing hydrogen silicone oil and 33.36g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil obtained by 50g and 64.07g allyl polyether, in 6ppm chloroplatinic acid catalyst and
Under the conditions of 100ppm diethanol amine co-catalyst, it is warming up to 120 DEG C under normal pressure, reacts 3h, obtains component A1, molecular formula are as follows:
Si(CH3)3-O-[Si(CH3)2-O]5·7-[Si(CH3)R-O]3·6-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)2(CH2CH(CH3)O)1CH3。
(2) component B1Synthesis
By 116.06g octamethylcy-clotetrasiloxane, 33.37g high containing hydrogen silicone oil and 30.57g hexamethyldisiloxane dense
Under effect of sulfuric acid, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil, 76.86g allyl polyether obtained by 40g, in 6ppm chloroplatinic acid catalyst and
Under the conditions of 100ppm diethanol amine co-catalyst, it is heated to 120 DEG C under normal pressure, reacts 3h, obtains component B1, molecular formula
Are as follows:
Si(CH3)3-O-[Si(CH3)2-O]7.8-[Si(CH3)R-O]2.6-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)2(CH2CH(CH3)O)6CH3。
(3) preparation of high rebound foam organic silicon surfactant
By component A1And B1With component C1(C1Make the polyether polyol of initiator, molecular weight 2000 for propylene glycol) it carries out
Different proportion mixes, and stirs 1h under the conditions of 30 DEG C of temperature, obtains high rebound foam organic silicon surfactant.
Embodiment 2:
(1) component A2Synthesis
By 88.13g octamethylcy-clotetrasiloxane, 39.09g high containing hydrogen silicone oil and 52.78g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil obtained by 55g and 53.29g allyl polyether, in 6ppm chloroplatinic acid catalyst and
Under the effect of 100ppm triethanolamine co-catalyst, normal heating is warming up to 110 DEG C of reaction 3.5h and obtains component A2, molecular formula are as follows:
Si(CH3)3-O-[Si(CH3)2-O]3.5-[Si(CH3)R-O]1.8-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)2(CH2CH(CH3)O)1CH3。
(2) component B2Synthesis
By 113.62g octamethylcy-clotetrasiloxane, 31.7g high containing hydrogen silicone oil and 34.68g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil, 73.05g allyl polyether obtained by 40g, in 6ppm chloroplatinic acid catalyst and
Under the effect of 100ppm triethanolamine co-catalyst, it is heated to 110 DEG C of reaction 3.5h under normal pressure and obtains component B2, molecular formula
Are as follows:
Si(CH3)3-O-[Si(CH3)2-O]6.8-[Si(CH3)R-O]2.2-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)2(CH2CH(CH3)O)6CH3。
(3) preparation of high rebound foam organic silicon surfactant
By component A1And B1With component C1(C1Make the polyether polyol of initiator, molecular weight 2000 for propylene glycol) it carries out
Different proportion mixes, and stirs 1h under the conditions of 30 DEG C of temperature, obtains high rebound foam organic silicon surfactant.
Embodiment 3:
(1) component A3Synthesis
By 91.59g octamethylcy-clotetrasiloxane, 43.26g high containing hydrogen silicone oil and 45.15g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil, 61.97g allyl polyether obtained by 48g, in 6ppm chloroplatinic acid catalyst and
Under the effect of 100ppm triethanolamine co-catalyst, 110 DEG C are heated under normal pressure, reaction 3.5h obtains component A3, molecular formula
Are as follows:
Si(CH3)3-O-[Si(CH3)2-O]4.2-[Si(CH3)R-O]2.3-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)3(CH2CH(CH3)O)1CH3。
(2) component B3Synthesis
By 109.46g octamethylcy-clotetrasiloxane, 42.36g high containing hydrogen silicone oil and 28.18g hexamethyldisiloxane dense
Under effect of sulfuric acid, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in containing hydrogen silicone oil obtained by 30g and 75.21g allyl polyether, in 6ppm chloroplatinic acid catalyst and
Under the effect of 100ppm triethanolamine co-catalyst, 110 DEG C are heated under normal pressure, reaction 3.5h obtains component B3, molecular formula
Are as follows:
Si(CH3)3-O-[Si(CH3)2-O]7.8-[Si(CH3)R-O]3.5-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)1(CH2CH(CH3)O)7CH3。
(3) preparation of high rebound foam organic silicon surfactant
By component A3And B3With component C3(C3Make the polyether polyol of initiator, molecular weight 2000 for propylene glycol) it carries out
Different proportion mixes, and stirs 1h under the conditions of 30 DEG C of temperature, obtains high rebound foam organic silicon surfactant.
Embodiment 4:
(1) component A4Synthesis
By 74.12g octamethylcy-clotetrasiloxane, 30.44g high containing hydrogen silicone oil and 75.44g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in 55g containing hydrogen silicone oil and 49.83g allyl polyether, in 6ppm chloroplatinic acid catalyst and 100ppm
Under the effect of triethanolamine co-catalyst, 110 DEG C of reaction 3.5h obtain component A4, molecular formula are as follows:
Si(CH3)3-O-[Si(CH3)2-O]2.1-[Si(CH3)R-O]1-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)3(CH2CH(CH3)O)1CH3。
(2) component B4Synthesis
By 109.63g octamethylcy-clotetrasiloxane, 39.4g high containing hydrogen silicone oil and 30.97g hexamethyldisiloxane in dense sulphur
Under acid effect, 30 DEG C of reaction 7h obtain containing hydrogen silicone oil.
Reactor is added in 32g containing hydrogen silicone oil, 74.61g allyl polyether, in 6ppm chloroplatinic acid catalyst and 100ppm tri-
Under the effect of ethanol amine co-catalyst, 110 DEG C are heated under normal pressure, reaction 3.5h obtains component B4, molecular formula are as follows:
Si(CH3)3-O-[Si(CH3)2-O]7.2-[Si(CH3)R-O]3-Si(CH3)3
Wherein, R=-CH2CH2CH2O(CH2CH2O)1(CH2CH(CH3)O)7CH3。
(3) preparation of high rebound foam organic silicon surfactant
By component A4And B4With component C4(C4Make the polyether polyol of initiator, molecular weight 2000 for propylene glycol) it carries out
Different proportion mixes, and stirs 1h under the conditions of 30 DEG C of temperature, obtains high rebound foam organic silicon surfactant.
In above-described embodiment 1-4, under the conditions of high rebound foam foaming formulation, obtains applying as shown in table 1- table 4 and comment
Valence result:
1 embodiment 1 of table compounds sample applicating evaluating result
Remarks: abscess thickness is represented with "+", and "+" increases that represent abscess thicker.
2 embodiment 2 of table compounds sample applicating evaluating result
Remarks: abscess thickness is represented with "+", and "+" increases that represent abscess thicker.
3 embodiment 3 of table compounds sample applicating evaluating result
Remarks: abscess thickness is represented with "+", and "+" increases that represent abscess thicker.
4 embodiment 4 of table compounds sample applicating evaluating result
Remarks: abscess thickness is represented with "+", and "+" increases that represent abscess thicker.
In the present embodiment, it can be obtained in conjunction with above-mentioned evaluation result, when component C ratio is fixed, the component C of different proportion is corresponding
System all has similar rule, and effective adjusting to abscess thickness may be implemented in the ratio by adjusting component A and component B,
The opening of polyurethane high resilience foam body and the balance of stability may be implemented, to meet high resilience polyurethane foam to body
Product, ventilation, shearing, surface and dimensional stability particular/special requirement, effective solution Miscibility and polyurethane foam
The problem of surface and dimensional stability.
The above, further embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, and it is any
Within the scope of the present disclosure, according to the technique and scheme of the present invention and its design adds those familiar with the art
With equivalent substitution or change, protection scope of the present invention is belonged to.
Claims (10)
1. a kind of high rebound foam organic silicon surfactant foams for polyurethane high resilience foam, which is characterized in that should
Surfactant is grouped as by tri- kinds of groups of A, B, C, wherein shown in the structural formula of component A following (1):
In structural formula (1): the value that the value of m is 2~15, n is 1~10, and the value of m+n is 3~15;
The structure of R are as follows:-CH2CH2CH2O(CH2CH2O)a(CH2CH(CH3)O)bR1, the value that wherein value of a is 1~7, b is 0~7, a
The value of+b is the alkyl that 1~10, R1 is 1~4 carbon atom number;
Wherein, shown in the structural formula following (2) of B component:
In structural formula (2): the value that the value of m is 1~25, n is 1~15, and the value of m+n is 2~25;
The structure of R are as follows:-CH2CH2CH2O(CH2CH2O)a(CH2CH(CH3)O)bR2, the value that the value of a is 0~20, b is 1~20, a+b
Value be alkyl that 1~20, R2 is 1~4 carbon atom number;
Wherein, component C is the copolymer with the terminal hydroxyl as derived from polyol.
2. a kind of high rebound foam organic silicon surfactant as described in claim 1, which is characterized in that the use of component A
Amount percentage is 20-40%, and the usage percentage of B component is 20-40%, and the usage percentage of component C is 20-60%.
3. a kind of high rebound foam organic silicon surfactant as described in claim 1, which is characterized in that component C is band
There is the copolymer of the terminal hydroxyl as derived from polyol, polyol is low molecular weight polyols, including second two
Alcohol, propylene glycol, 1,3 butylene glycol, 1,4- butanediol, 1,6-HD, neopentyl glycol, diethylene glycol (DEG) and dipropylene glycol.
4. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in any one of claims 1-3,
It is characterized by comprising the following steps:
Step 1: containing hydrogen silicone oil preparation
Using octamethylcy-clotetrasiloxane, high containing hydrogen silicone oil and hexamethyldisiloxane as raw material, under acidic catalyst effect,
Under the conditions of reaction temperature is 30~90 DEG C, 5~8h is reacted, the containing hydrogen silicone oil of different structure is obtained;
Step 2: the preparation of component A and component B
Allyl polyether, chloroplatinic acid catalyst, the co-catalyst of above-mentioned resulting at least one containing hydrogen silicone oil and different structure add
Enter in reactor, normal pressure is warming up to 90-160 DEG C, reacts 2~8h, obtains two kinds of organic silicon modified by polyether surfactants: component
A and B;
Step 3: the preparation of high rebound foam organic silicon surfactant
Resulting component A and B and component C are mixed according to different weight ratio, obtain high rebound foam organosilicon table
Face activating agent.
5. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 4, which is characterized in that
In step 1, acidic catalyst is at least one of Emathlite, sulfuric acid, trifluoromethanesulfonic acid and acidic resins.
6. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 5, which is characterized in that
Acidic catalyst is sulfuric acid, and dosage is the 1~2% of quality of material used.
7. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 4, which is characterized in that
In step 2, chloroplatinic acid catalyst is platinum catalyst, and platinum dosage is the 3-20ppm of material total amount.
8. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 4, which is characterized in that
In step 2, co-catalyst is at least one of diethanol amine, triethanolamine, acetamide, triethylamine and N- butylethanolamine.
9. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 8, which is characterized in that
Co-catalyst dosage is 3~80ppm of material total amount.
10. a kind of preparation method of high rebound foam organic silicon surfactant as claimed in claim 4, feature exist
In in step 3, the weight percent of component A is 20-40%, and the weight percent of component B is 20-40%, the weight of component C
Percentage is 20-60%.
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CN113317315A (en) * | 2021-05-31 | 2021-08-31 | 浙江润禾有机硅新材料有限公司 | Low-foam organic silicon surfactant and preparation method and application thereof |
CN113317315B (en) * | 2021-05-31 | 2022-06-24 | 浙江润禾有机硅新材料有限公司 | Low-foam organic silicon surfactant and preparation method and application thereof |
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