CN103740112B - A kind of seepage-proof oil silicon gel of filling for chest pad and preparation method thereof - Google Patents
A kind of seepage-proof oil silicon gel of filling for chest pad and preparation method thereof Download PDFInfo
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- CN103740112B CN103740112B CN201310738165.4A CN201310738165A CN103740112B CN 103740112 B CN103740112 B CN 103740112B CN 201310738165 A CN201310738165 A CN 201310738165A CN 103740112 B CN103740112 B CN 103740112B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 55
- 239000010703 silicon Substances 0.000 title claims abstract description 55
- 239000003921 oil Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 239000003112 inhibitor Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 38
- 229920000642 polymer Polymers 0.000 claims description 34
- -1 siloxanes Chemical class 0.000 claims description 27
- 229910052697 platinum Inorganic materials 0.000 claims description 19
- 238000012545 processing Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 2
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical compound CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 claims description 2
- 229960002238 methylpentynol Drugs 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000499 gel Substances 0.000 description 43
- 239000011159 matrix material Substances 0.000 description 7
- 230000035515 penetration Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 0 C*N*N[Si](*C)(*O*)C(C)=C Chemical compound C*N*N[Si](*C)(*O*)C(C)=C 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- LDTAOIUHUHHCMU-UHFFFAOYSA-N 3-methylpent-1-ene Chemical group CCC(C)C=C LDTAOIUHUHHCMU-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229920006037 cross link polymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000004132 cross linking Methods 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
- 239000003085 diluting agent Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000004519 manufacturing process 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
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 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
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of seepage-proof oil silicon gel of filling for chest pad and preparation method thereof, the composition of raw materials of this seepage-proof oil silicon gel is counted by weight, is made up of 96～105 base-materials, 5～10 parts of crosslinking agents, 0.05～0.15 part of catalyst and 0.05 part of inhibitor. Seepage-proof oil silicon gel of the present invention, has the advantages that pliability is good and plasticity is high, and when filling as chest pad, sense of touch is good, and oil-tight.
Description
Technical field
The present invention relates to chest pad material technology field, relate in particular to chest pad filling and use silicon gel, be specifically related to a kind of chest padFill seepage-proof oil silicon gel of use and preparation method thereof.
Background technology
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 for chest pad fill, there is pliabilityGood, 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 seepage-proof oil silicon gel of filling for chest pad, its composition of raw materials is the each component group by following parts by weightBecome:
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=100～150;
In above-mentioned formula (II), b=45～50;
In above-mentioned formula (I) and formula (II), R1For vinyl, 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 diluent, and linear siloxanes polymer difference and the non-reactive group shown in general formula (II)Group's silicone oil, it does not participate in being cross-linked, and can become key with crosslinked and 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 3:1～1:1; 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 3:1, 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 1:1, 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 3:1～1:1.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), m=8～12, n=3～6.
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 adopts any commercially available platinum catalyst all can realize the present invention; PreferablyKarst platinum catalyst [chemical name is platinum (O) divinyl tetramethyl disiloxane solution], platinum content is3000pmm; Because the inventor is by carrying out multiple platinum catalyst, classification experiment is rear to be found, Karst platinum catalystActivity is the highest, and best with the compatibility of base-material of the present invention.
Will there is curing reaction in base-material, crosslinking agent and catalyst in the present invention's formula, cause in mixed processFinished product is just difficult to obtain required shape and proterties, and solidifies inhomogeneous, therefore, before solidification temperature does not reach, necessary logicalCross and add inhibitor to suppress the generation of curing reaction under room temperature, in above-mentioned raw materials formula, inhibitor plays this inhibition work exactlyWith, thereby the complexing body that inhibitor can generate certain forms with platinum catalyst is realized inhibitory action; The inventor forThe feature of the present invention's formula, the inhibitor that plurality of optional is selected is optimized, and final inhibitor selects to adopt alkynol class inhibitor,Because alkynol class inhibitor is the inhibitor of a class volatile, under solidification temperature of the present invention, can vapor away well,Thereby curing reaction carries out, and inhibitor itself can not impact the final performance of product; Inhibitor of the present invention adopts commercially availableAny alkynol class inhibitor all can realize the present invention, preferably 1-butine-3-alcohol, methylpentynol or 3,5-Dimethyl-1-hexin-3-alcohol.
The inventor is also optimized the composition of raw materials of above-mentioned a kind of seepage-proof oil silicon gel of filling for chest pad, asShown in lower:
The present invention also provides the preparation method of above-mentioned a kind of seepage-proof oil silicon gel of filling for chest pad, this preparation method's bagDraw together following steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumizing and defoamingRear pouring, is then cured processing, prepares required seepage-proof oil silicon gel of filling for chest pad.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
In above-mentioned preparation method, solidifying processing temperature used is 85 DEG C～150 DEG C, preferably 120 DEG C, because the inventorFind by research, if solidification temperature, lower than 85 DEG C, needs hardening time more of a specified duration, and long being unfavorable for finally of hardening timeThe raising of production capacity, if solidification temperature higher than 150 DEG C, solidifying time reaction can be very violent, and violent reaction can make in colloidProduce a large amount of bubbles, thereby affect the quality of product.
In above-mentioned preparation method, be 20min～35min hardening time, preferably 30min.
A kind of seepage-proof oil silicon gel of filling for chest pad of the present invention, not only pliability is good, plasticity is high for it, and notCan oil impregnate.
Compared with prior art, the present invention has the following effect of having a mind to:
1. a kind of seepage-proof oil silicon gel of filling for chest pad of the present invention, the base-material in its composition of raw materials, adopts two endsFor linear siloxanes polymer and one end of unsaturated bond are that the unsaturated bond other end is the linear siloxanes polymer of saturated bondCollocation forms, and has optimized both ratios, therefore can realize well not only good, the plasticity of pliability of final silicon gelHeight, and oil-tight;
2. a kind of seepage-proof oil silicon gel of filling for chest pad of the present invention, the crosslinking agent in its composition of raw materials, catalystAll for base-material and goal of the invention and optimize screening, therefore, can ensure well the soft of final silicon gel with inhibitorGood toughness, plasticity are high, and oil-tight;
3. a kind of seepage-proof oil silicon gel of filling for chest pad of the present invention, it is with low cost, and preparation method is simple, is used asWhen chest pad is filled, sense of touch 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
The silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
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=50;
In above-mentioned formula (I) and formula (II), R1For vinyl, 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 3:1.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), m=9, n=6.
In above-mentioned raw materials formula, catalyst is Karst platinum catalyst, and platinum content is 3000pmm; Inhibitor is 3,5-dimethyl-1-hexin-3-alcohol.
The preparation method of the present embodiment silicon gel, specifically comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumizing and defoamingRear pouring, is then cured processing, prepares the silicon gel of the present embodiment.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
In above-mentioned preparation method, solidifying processing temperature used is 85 DEG C, and be 35min hardening time.
Embodiment 2
The silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
In above-mentioned raw materials formula, this base-material is linear siloxanes polymer and the structural formula as shown in general formula (I) by structural formulaLinear siloxane polymer as shown in general formula (II) forms:
In above-mentioned formula (I), a=120;
In above-mentioned formula (II), b=48;
In above-mentioned formula (I) and formula (II), R1For vinyl, 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 1:1.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), m=8, n=4.
In above-mentioned raw materials formula, catalyst is Karst platinum catalyst, and platinum content is 3000pmm; Inhibitor is 1-Butine-3-alcohol.
The preparation method of the present embodiment silicon gel, specifically comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumizing and defoamingRear pouring, is then cured processing, prepares the silicon gel of the present embodiment.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
In above-mentioned preparation method, solidifying processing temperature used is 150 DEG C, and be 20min hardening time.
Embodiment 3
The silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
In above-mentioned raw materials formula, this base-material is linear siloxanes polymer and the structural formula as shown in general formula (I) by structural formulaLinear siloxane polymer as shown in general formula (II) forms:
In above-mentioned formula (I), a=150;
In above-mentioned formula (II), b=45;
In above-mentioned formula (I) and formula (II), R1For vinyl, 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 2:1.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (III):
In above-mentioned formula (III), m=12, n=3.
In above-mentioned raw materials formula, catalyst is Karst platinum catalyst, and platinum content is 3000pmm; Inhibitor is 3-Methyl-1-pentene alkynes-3-alcohol.
The preparation method of the present embodiment silicon gel, specifically comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumizing and defoamingRear pouring, is then cured processing, prepares the silicon gel of the present embodiment.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
In above-mentioned preparation method, solidifying processing temperature used is 120 DEG C, and be 30min hardening time.
Comparative example 1
The silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
In above-mentioned raw materials formula, this base-material is the linear siloxanes polymer shown in general formula (I):
In above-mentioned formula (I), a=150;
In above-mentioned formula (I), R1For vinyl.
In above-mentioned raw materials formula, the structural formula of crosslinking agent is as shown in general formula (II):
In above-mentioned formula (II), m=12, n=3.
In above-mentioned raw materials formula, catalyst is Karst platinum catalyst, and platinum content is 3000pmm; Inhibitor is 3-Methyl-1-pentene alkynes-3-alcohol.
The preparation method of the present embodiment silicon gel, specifically comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumizing and defoamingRear pouring, is then cured processing, prepares the silicon gel of the present embodiment.
In above-mentioned preparation method, the vacuum that vacuumizing and defoaming adopts is-0.095Mpa.
In above-mentioned preparation method, solidifying processing temperature used is 120 DEG C, and be 30min hardening time.
Comparative example 2
The silicon gel of the present embodiment, its composition of raw materials is made up of the each component of following parts by weight:
In above-mentioned raw materials formula, this base-material is that the linear siloxane polymer shown in general formula (I) forms:
In above-mentioned formula (I), b=45;
In above-mentioned formula (I), R1For vinyl, 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), m=12, n=3.
In above-mentioned raw materials formula, catalyst is Karst platinum catalyst, and platinum content is 3000pmm; Inhibitor is 3-Methyl-1-pentene alkynes-3-alcohol.
The preparation method of the present embodiment silicon gel, specifically comprises the steps:
According to above-mentioned formula, by first to matrix, crosslinking agent, catalyst and inhibitor mixing and stirring, then vacuumize (vacuumDegree is-0.095Mpa) water after deaeration, be then cured processing, liquid 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 penetration number of embodiment 1-3 is larger, illustrates that the pliability of silicon gel is good, and oil-tight,Although and comparative example 1 is also oil-tight, its penetration number is less than normal, therefore much higher hard, is not suitable for use in chest pad and fillsThing.
Claims (5)
- For chest pad fill a seepage-proof oil silicon gel, the composition of raw materials that it is characterized in that this seepage-proof oil silicon gel be by asThe each component composition of lower parts by weight: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 formulaShape siloxane polymer forms:In above-mentioned formula (I), a=100～150;In above-mentioned formula (II), b=45～50;In above-mentioned formula (I) and formula (II), R1For vinyl, R2For methyl;Shown in linear siloxanes polymer shown in above-mentioned general formula (I) and general formula (II), the weight ratio of linear siloxanes polymer is 3:1～1:1；The structural formula of above-mentioned crosslinking agent is as shown in general formula (III):In above-mentioned formula (III), m=8～12, n=3～6;Described catalyst is Karst platinum catalyst, and platinum content is 3000ppm;Described inhibitor is 1-butine-3-alcohol, methylpentynol or 3,5-dimethyl-1-hexin-3-alcohol.
- 2. a preparation method for the seepage-proof oil silicon gel of filling for chest pad described in claim 1, is characterized in that this preparationMethod comprises the steps:By first to base-material, crosslinking agent, catalyst and inhibitor mixing and stirring, then water after vacuumizing and defoaming, then consolidateChange and process, prepare required seepage-proof oil silicon gel of filling for chest pad.
- 3. the preparation method of the seepage-proof oil silicon gel of filling for chest pad according to claim 2, takes out described in it is characterized in thatThe vacuum that vacuum defoamation adopts is-0.095MPa.
- 4. the preparation method of the seepage-proof oil silicon gel of filling for chest pad according to claim 2, is characterized in that described solidChanging processing temperature used is 85 DEG C～150 DEG C, and be 20min～35min hardening time.
- 5. the preparation method of the seepage-proof oil silicon gel of filling for chest pad according to claim 4, is characterized in that described solidChanging processing temperature used is 120 DEG C, and be 30min hardening time.
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