CN103756326B - A kind of seepage-proof oil silicon gel and preparation method thereof - Google Patents
A kind of seepage-proof oil silicon gel and preparation method thereof Download PDFInfo
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- CN103756326B CN103756326B CN201310738296.2A CN201310738296A CN103756326B CN 103756326 B CN103756326 B CN 103756326B CN 201310738296 A CN201310738296 A CN 201310738296A CN 103756326 B CN103756326 B CN 103756326B
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 53
- 239000010703 silicon Substances 0.000 title claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000003921 oil Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000001879 gelation Methods 0.000 title abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims description 36
- -1 siloxanes Chemical class 0.000 claims description 28
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- DGYMCGCIUWHSNH-UHFFFAOYSA-N C(CCC)[Sn]CCCC.C(CCCCCCCCCCC)[S] Chemical compound C(CCC)[Sn]CCCC.C(CCCCCCCCCCC)[S] DGYMCGCIUWHSNH-UHFFFAOYSA-N 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical group CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 2
- 150000002148 esters Chemical class 0.000 claims 2
- 239000000499 gel Substances 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 description 5
- 230000035515 penetration Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000012974 tin catalyst Substances 0.000 description 1
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- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of seepage-proof oil silicon gel and preparation method thereof, and the composition of raw materials of this seepage-proof oil silicon gel is made up of the each component of following parts by weight: 0.05～0.15 part of 100 parts of base-materials, 1～2 part of crosslinking agent and catalyst. When seepage-proof oil silicon gel of the present invention is filled as chest pad, sense of touch is good, and pliability is good, and plasticity is high, oil-tight, and with low cost, and preparation method is simple, has very high economic worth.
Description
Technical field
The present invention relates to chest pad material technology field, relate in particular to chest pad and fill and use silicon gel, be specifically related to one passableAs seepage-proof oil silicon gel of chest pad filler and preparation method thereof.
Background technology
Everybody has a love of beauty, and chest pad can play the effect that beautifies chest effectively, is therefore subject to wide all the timeLarge women likes, and market is boundless. Chest pad filler has a variety of, and silicon gel is the one of wherein relatively commonly using.
Silicon gel is that a kind of low viscosity, band viscosity, gel are transparent, dual composition addition type silicon gel, can room temperatureSolidify, also can be heating and curing, have that temperature is higher solidifies faster feature, silicon gel be mainly used in body configuration, sexual organ,The flexible silica gel products such as chest pad, shoulder pad, paster, slipmat.
Inventor is filled and is investigated with silicon gel by the chest pad to selling on market, found that, current on marketThe chest pad filler silicon gel generally using, has that elasticity is bad, flexibility is very poor or contains the problems such as oil is serious, and useThe feel of getting up is bad, uses extremely inconvenient while especially containing oil. Although some product pliability is good, elasticity is bad and easily depositIn the oily phenomenon of a large amount of Sheng, otherwise, although some product has certain elasticity, do not contain oil, its pliability is non-constant, because ofThis, the product on existing market cannot be realized elasticity, pliability and all features of while of three performances of anti-Sheng oil.
As can be seen here, how to develop that not only pliability is good, elasticity is good and can not contain oily chest pad and fill and use silicon gelBe the problem that the industry need solve, there is very large challenge, and there is very high market value.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of can be used for chest pad fill, have pliable and toughProperty is good, elasticity is good and the silicon gel of seepage-proof oil feature.
Another object of the present invention is to provide the preparation method of above-mentioned silicon gel.
Above-mentioned purpose of the present invention is achieved by following scheme:
A kind of seepage-proof oil silicon gel, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
1～2 part of crosslinking agent;
0.05～0.15 part of catalyst.
Above-mentioned raw materials formula preferred version is as follows:
100 parts of base-materials;
1.9 parts of crosslinking agents;
0.1 part of catalyst.
Base-material, as the main component of silicon gel, has determined the performance of silicon gel to a great extent, therefore, and in order to realize thisThe object of invention, the inventor finds by research: if the two ends of base-material structural formula are all unsaturated bond, final colloid is strongSpend high, but plasticity is not strong; If the two ends of base-material structural formula are all saturated bond, although plasticity is strong, easily occurOil impregnate; Therefore,, by after plurality of optional being selected to base-material and studying and screen, the inventor obtains realizing the object of the inventionBase-material, this base-material by structural formula the linear siloxanes polymer as shown in general formula (I) and structural formula as shown in general formula (II)Linear siloxane polymer forms:
In above-mentioned formula (I), a=100;
In above-mentioned formula (II), b=200～300;
In above-mentioned formula (I) and formula (II), R1For hydroxyl, R2For methyl.
In above-mentioned base-material, the linear siloxanes polymer shown in general formula (I), its two ends are unsaturated bond, and main rising carriedFor the effect of base-material crosslinked; Linear siloxanes polymer shown in general formula (II), its one end is unsaturated bond, one end is saturatedKey, mainly plays plasticizer, and the linear siloxanes polymer shown in general formula (II) is different and nonactive group silicone oil, itDo not participate in being cross-linked, can become key with crosslinked and not ooze out, also can single-ended Cheng Jian, so can not ooze out.
In above-mentioned base-material, linear siloxanes polymer shown in linear siloxanes polymer shown in general formula (I) and general formula (II)Weight ratio be 1:2～1:4; Because inventor finds by research, if linear siloxanes polymer shown in general formula (I) and logicalWhen shown in formula (II), the weight ratio of linear siloxanes polymer is greater than 1:2, the linear siloxanes polymer of plasticizationComponent is on the low side, can cause the pliability of final silicon gel poor, and sense of touch is uncomfortable; And if linear siloxanes polymerization shown in general formula (I)Shown in thing and general formula (II), the weight ratio of linear siloxanes polymer is less than: when 1:4, play crosslinked unsaturated point inclined to one sideFew, can cause final silicon gel for liquid, or easy oil impregnate; Therefore, the inventor passes through two kinds of linear siloxanes in base-materialAfter the dosage optimization of polymer, selection optimum weight ratio is 1:2～1:4.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), R is any one in methyl, ethyl, propyl group or butyl.
The effect of above-mentioned crosslinking agent is for matrix provides bridge formation, makes the mutual bonding cross-linking of multiple linear molecules reticulate knotStructure.
In above-mentioned raw materials formula, catalyst adopt commercially available any organotin catalysts or titanium complex catalyst equalCan realize the present invention, as dibutyltin dilaurate, stannous octoate, two (dodecyl sulphur) dibutyl tin or butyl titanate,Preferably dibutyltin dilaurate
In above-mentioned raw materials formula, because linear siloxanes polymer shown in base-material formula of (I) and general formula (II) institute timberlineIn shape siloxane polymer, having one end at least is carboxyl, and therefore, the preparation process of this silicon gel is condensed type, and condensed type beUnder room temperature, by absorbing airborne moisture generation cross-linking reaction, himself reaction is just slow, therefore suppresses without adoptingAgent.
The present invention also provides the preparation method of above-mentioned a kind of seepage-proof oil silicon gel, and this preparation method comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent and catalyst mixing and stirring, then after vacuumizing and defoaming, room temperatureSolidify 3 hours, prepare required with seepage-proof oil silicon gel.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
Compared with prior art, the present invention has the following effect of having a mind to:
1. seepage-proof oil silicon gel of the present invention, the base-material in its composition of raw materials, adopts the linear silicon that two ends are unsaturated bondOxygen alkane polymer and one end are that the unsaturated bond other end is that the linear siloxanes polymer collocation of saturated bond forms, and have optimizedBoth ratios, not only pliability is good, plasticity is high therefore can to realize well final silicon gel, and oil-tight;
2. seepage-proof oil silicon gel of the present invention, the base-material in its composition of raw materials, end is hydroxyl, therefore curing reaction is contractingClose reaction, so without using inhibitor, and catalyst is also without adopting expensive platinum catalyst, adopts cheap havingMachine tin catalyst or titanium complex catalyst, cost reduces greatly;
3. seepage-proof oil silicon gel of the present invention, it is with low cost, and preparation method is simple, sense of touch when filling as chest padGood, pliability is good, oil-tight, therefore has very high economic worth.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is done further and described, but specific embodiment is not appointed the present inventionWhat limits.
Embodiment 1
A kind of seepage-proof oil silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
2 parts of crosslinking agents;
0.05 part of catalyst.
In above-mentioned raw materials formula, base-material by structural formula the linear siloxanes polymer as shown in general formula (I) and structural formula asLinear siloxane polymer shown in general formula (II) forms:
In above-mentioned formula (I), a=100;
In above-mentioned formula (II), b=200;
In above-mentioned formula (I) and formula (II), R1For hydroxyl, R2For methyl.
In above-mentioned base-material, linear siloxanes polymer shown in linear siloxanes polymer shown in general formula (I) and general formula (II)Weight ratio be 1:3.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), R is methyl.
In above-mentioned raw materials formula, catalyst is stannous octoate.
The preparation method of above-mentioned a kind of seepage-proof oil silicon gel, this preparation method comprises the steps:
According to above-mentioned formula, by matrix, crosslinking agent and the first mixing and stirring of catalyst, then vacuumize (vacuum for-0.095Mpa) after deaeration, cold curing 3 hours, prepares the seepage-proof oil silicon gel of the present embodiment.
Embodiment 2
A kind of seepage-proof oil silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
1 part of crosslinking agent;
0.14 part of catalyst.
In above-mentioned raw materials formula, base-material by structural formula the linear siloxanes polymer as shown in general formula (I) and structural formula asLinear siloxane polymer shown in general formula (II) forms:
In above-mentioned formula (I), a=100;
In above-mentioned formula (II), b=300;
In above-mentioned formula (I) and formula (II), R1For hydroxyl, R2For methyl.
In above-mentioned base-material, linear siloxanes polymer shown in linear siloxanes polymer shown in general formula (I) and general formula (II)Weight ratio be 1:2.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), R is propyl group.
In above-mentioned raw materials formula, catalyst is butyl titanate.
The preparation method of above-mentioned a kind of seepage-proof oil silicon gel, this preparation method comprises the steps:
According to above-mentioned formula, by matrix, crosslinking agent and the first mixing and stirring of catalyst, then vacuumize (vacuum for-0.095Mpa) after deaeration, cold curing 3 hours, prepares the seepage-proof oil silicon gel of the present embodiment.
Embodiment 3
A kind of seepage-proof oil silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
1.9 parts of crosslinking agents;
0.1 part of catalyst.
In above-mentioned raw materials formula, base-material is that the linear siloxanes polymer shown in general formula (I) and structural formula are as general formula (II)Shown linear siloxane polymer forms:
In above-mentioned formula (I), a=100;
In above-mentioned formula (II), b=250;
In above-mentioned formula (I) and formula (II), R1For hydroxyl, R2For methyl.
In above-mentioned base-material, linear siloxanes polymer shown in linear siloxanes polymer shown in general formula (I) and general formula (II)Weight ratio be 1:4.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), R is ethyl.
In above-mentioned raw materials formula, catalyst is dibutyltin dilaurate.
The preparation method of above-mentioned a kind of seepage-proof oil silicon gel, this preparation method comprises the steps:
According to above-mentioned formula, by matrix, crosslinking agent and the first mixing and stirring of catalyst, then vacuumize (vacuum for-0.095Mpa) after deaeration, cold curing 3 hours, prepares the seepage-proof oil silicon gel of the present embodiment.
Comparative example 1
A kind of seepage-proof oil silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
1.9 parts of crosslinking agents;
0.1 part of catalyst.
In above-mentioned raw materials formula, base-material is the linear siloxanes polymer shown in general formula (I):
In above-mentioned formula (I), a=100;
In above-mentioned formula (I), R1For hydroxyl.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (II):
In above-mentioned formula (II), R is ethyl.
In above-mentioned raw materials formula, catalyst is dibutyltin dilaurate.
The preparation method of above-mentioned a kind of seepage-proof oil silicon gel, this preparation method comprises the steps:
According to above-mentioned formula, by matrix, crosslinking agent and the first mixing and stirring of catalyst, then vacuumize (vacuum for-0.095Mpa) after deaeration, cold curing 3 hours, prepares the seepage-proof oil silicon gel of the present embodiment.
Comparative example 2
A kind of seepage-proof oil silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
100 parts of base-materials;
1.9 parts of crosslinking agents;
0.1 part of catalyst.
In above-mentioned raw materials formula, base-material is the linear siloxanes polymer shown in general formula (I):
In above-mentioned formula (I), b=250;
In above-mentioned formula (I), R1For hydroxyl, R2For methyl.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (II):
In above-mentioned formula (II), R is ethyl.
In above-mentioned raw materials formula, catalyst is dibutyltin dilaurate.
The preparation method of above-mentioned a kind of seepage-proof oil silicon gel, this preparation method comprises the steps:
According to above-mentioned formula, by matrix, crosslinking agent and the first mixing and stirring of catalyst, then vacuumize (vacuum for-0.095Mpa) after deaeration, cold curing 3 hours, cannot solidify.
Embodiment 4 performance tests
Carrying out property of silicon gel prepared by embodiment 1, embodiment 2, embodiment 3, comparative example 1 and comparative example 2Can test, mainly comprise pliability and the whether test of two aspects of oil impregnate.
(1) flexible test adopts the method for needle penetration
Needle penetration refers to that, in certain load degree of depth of penetrating in grease sample vertical with time internal standard pin, needle penetration numerical value moreGreatly, show that this grease is softer, mechanical strength is lower. In the time that crosslinked polymer degree density increases, mechanical strength also can increase, polymerizationThe needle penetration numerical value of thing declines; In the time that crosslinked polymer degree density reduces, mechanical strength is corresponding decline also, thereupon the pin of polymerIn-degree numerical value rises. So carry out the crosslink density of characterize polymers herein by measuring the needle penetration numerical value of polymer. Pin entersNumber of degrees value greatly crosslink density is low, otherwise crosslink density is high.
(2) silicon gel oil impregnate detection method;
At room temperature the silicon gel of curing molding is placed on white filter paper, leaves standstill 24 hours, then visually observe filter paper, seeWhether there is oil diffusion to determine whether oil impregnate of silicon gel.
The performance test results is as shown in table 1:
Table 1 the performance test results
As can be seen from Table 1, the pliability of embodiment 1-3 is all good, and oil-tight, and comparative example 1 pliabilityVery poor, hardness is high, and 2 of comparative examples cannot be solidified completely.
Claims (4)
1. a seepage-proof oil silicon gel, is characterized in that the composition of raw materials of described seepage-proof oil silicon gel is by following parts by weightEach component composition:
100 parts of base-materials;
1.9 parts of crosslinking agents;
0.1 part of catalyst;
Above-mentioned base-material is the linear siloxanes polymer as shown in general formula (I) and the line of structural formula as shown in general formula (II) by structural formulaProperty siloxane polymer form:
In above-mentioned formula (I), a=100;
In above-mentioned formula (II), b=200～300;
In above-mentioned formula (I) and formula (II), R1For hydroxyl, R2For methyl;
The weight ratio of linear siloxanes polymer shown in linear siloxanes polymer shown in general formula (I) and general formula (II) be 1:2～1:4；
The structural formula of above-mentioned crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), R is any one in methyl, ethyl, propyl group or butyl.
2. a kind of seepage-proof oil silicon gel according to claim 1, is characterized in that described catalyst is dibutyl tin two baysAcid esters, stannous octoate, two (dodecyl sulphur) dibutyl tin or butyl titanate.
3. a kind of seepage-proof oil silicon gel according to claim 2, is characterized in that described catalyst is dibutyl tin two baysAcid esters.
4. a preparation method for a kind of seepage-proof oil silicon gel of any one described in claim 1-3, is characterized in that this preparationMethod comprises the steps:
By first to matrix, crosslinking agent and catalyst mixing and stirring, then after vacuumizing and defoaming, cold curing 3 hours, is prepared intoTo the required seepage-proof oil silicon gel of using; The vacuum that described vacuumizing and defoaming adopts is-0.095Mpa.
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| US4551516A (en) * | 1983-05-17 | 1985-11-05 | Toray Industries, Inc. | Coating composition and the use thereof |
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