CN1572835A - Rubber composition for roller and ionic conductive rubber roller using the composition - Google Patents
Rubber composition for roller and ionic conductive rubber roller using the composition Download PDFInfo
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- CN1572835A CN1572835A CNA2004100451892A CN200410045189A CN1572835A CN 1572835 A CN1572835 A CN 1572835A CN A2004100451892 A CNA2004100451892 A CN A2004100451892A CN 200410045189 A CN200410045189 A CN 200410045189A CN 1572835 A CN1572835 A CN 1572835A
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- thiazolinyl
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- polyoxyalkylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
- C09D171/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention provides an addition-curable rubber composition suitable for manufacturing a rubber for a roll that is free of the tackiness of the rubber surface and oil bleeding and used for electrophotographic image forming apparatuses and the like. The addition-curable rubber composition for the roll contains (A) a polyoxyalkylene having at least two alkenyl groups in the molecule, (B) an organopolysiloxane having at least two alkenyl groups and containing 10-50 mol% of phenyl groups bonded to silicon atoms based on the total organic groups bonded to the silicon atoms, (C) an organohydrogenpolysiloxane having in the molecule at least two hydrogen atoms bonded to silicon atoms, (D) a platinum catalyst, and (E) an ion conductivity imparting agent.
Description
Technical field
The present invention relates to be used for roller the addition curable rubber combination and the ionic conductivity rubber coated pressure bowl of electro photography image processing system.
Background technology
In JP7-300564A, put down in writing to containing and solidifying as main component, by hydrosilylation reactions with polyoxyalkylene to add in the addition curable rubber combination of gained and given the compound of said composition electroconductibility, and used resulting composition to make the method for ionic conductivity rubber coated pressure bowl.According to this method, make the ionic conductivity rubber coated pressure bowl by around roller, solidifying said composition and form the ionic conductivity rubber layer.
But,, use very difficulty as rubber coated pressure bowl because gained ionic conductivity rubber coated pressure bowl exists its rubber surface to have tackiness (viscosity), unreacted polymkeric substance from problems such as this rubber surface oil ooze.
Summary of the invention
The addition curable rubber combination that problem of the present invention provides is that the tackiness that do not have rubber surface and oil ooze, be suitable for rubber manufacturing at the roller that is used for electro photography image processing system etc.In addition, be provided at the ionic conductivity rubber coated pressure bowl that the roller axle is provided with the ionic conductivity rubber layer on every side.
In order to solve above-mentioned problem, the invention provides roller addition curable rubber combination, this rubber combination contains
(A) in a molecule, contain the polyoxyalkylene of 2 thiazolinyls at least: 100 weight parts
(B) in a molecule, have 2 at least with general formula (1):
R
1 aR
2 bSiO
(4-a-b)/2(1)
(in the formula, R
1The expression thiazolinyl, R
2Identical or different, expression does not have the 1 valency alkyl aliphatics unsaturated link(age), non-replacement or replacement, a is 1 or 2, b is the integer of 0-2, but, a+b is the integer of 1-3) organopolysiloxane that contains thiazolinyl of siloxane unit of expression: the 20-200 weight part, wherein contain account for the whole organic group 10-50mol% of Siliciumatom bonded with Siliciumatom bonded phenyl
(C) with an average group accepted way of doing sth (2):
R
3 cH
dR
4 eSiO
(4-c-d-e)/2????(2)
(in the formula, R
3The expression phenyl, R
4Represent except that phenyl, do not have the aliphatics unsaturated link(age), 1 valency alkyl of non-replacement or replacement, c is the number of 0＜c≤2, d is the number of 0＜d≤1, e is the number of 0≤e＜2, but, c+d+e is the number of 0.7＜c+d+e≤3) expression, at least contain 2 organic hydride diene (Ha イ De ロ ジ エ Application) polysiloxane with Siliciumatom bonded hydrogen atom in a molecule: its content is for making in (C) component that contained and Siliciumatom bonded hydrogen atom are the amount of 0.1-3.0 with respect to the mol ratio of contained thiazolinyl at (A) and (B)
(D) platinum group catalyst: significant quantity,
And
(E) ionic conductivity imparting agent: 0.5-10 weight part.
In addition, the invention provides the ionic conductivity rubber coated pressure bowl of the ionic conductivity rubber layer that has core and form by the cured article that covers the above-mentioned rubber combination around this core.
The working of an invention mode
Below, invention is described in detail.
(addition curable rubber combination)
Rubber combination of the present invention is the material that contains above-mentioned (A)-(E) component.So, the each component that constitutes this rubber combination is described.
-(A) contain the polyoxyalkylene of thiazolinyl-
The polyoxyalkylene that contains thiazolinyl as the present invention (A) component can be known polyoxyalkylene (a so-called polyethers), for example, remove the terminal group of molecular chain, the about 100 moles of % (that is 95-100 mole %) that constitute backbone units are the polymers that is made of the olefin oxide unit.As these object lessons, can enumerate polyoxypropylene, polyoxyethylene, poly-(ethylene oxide propylene oxide) interpolymer etc., preferably can enumerate polyoxypropylene.
(A) have 2, preferred 2-10, preferred especially 2-4 thiazolinyl in molecule of component at least.This thiazolinyl can be positioned at the non-end of molecular chain, terminal or above two kinds of positions of molecular chain.Especially this thiazolinyl is present in molecular chain two ends of the polyoxyalkylene of (A) component at least,, preferably is present in the two terminal or be present in non-terminal two kinds of positions of two ends and the molecular chain of molecular chain of molecular chain that is.This thiazolinyl is that carbonatoms is preferably 2-8, is preferably the thiazolinyl of 2-6 especially.As its concrete example, can enumerate vinyl, allyl group, propenyl, pseudoallyl, butenyl etc., preferably can enumerate vinyl, allyl group.
(A) molecular weight of component represents to be generally 1 with number-average molecular weight, 000-50, and 000, be preferably 5,000-30,000.If this number-average molecular weight satisfies 5,000-30 in 000 the scope, can obtain at aspects such as physical strength, solidified nature excellent especially rubber combination.
Aforesaid (A) component can be used general formula:
(in the formula, X is H or CH independently
3, respectively the do for oneself integer of 0-2 of s, t is the integer of 2-4, n be 2 or above, be preferably 2-1,000, the integer of 2-500 more preferably) expression.As its concrete example, can enumerate
(in the formula, m and n respectively do for oneself 2 or above, be preferably 2-1,000, the integer of 2-500 more preferably) etc.
(A) component can a kind of independent use, also can 2 kinds or be used in combination more.
In addition, present inventors find, in order to suppress the gained curing rubber (promptly, the material that solidifies rubber combination of the present invention and obtain) to the rising of resistance value of energising voltage, with number-average molecular weight be 5,000 or the above polyoxyalkylene that contains thiazolinyl (a) and number-average molecular weight be 500 or the following polyoxyalkylene that contains thiazolinyl (b) coupling be effective.The proportion optimization of this polyoxyalkylene (a) and polyoxyalkylene (b) respectively do for oneself 50-98 weight % and 2-50 weight %, more preferably 50-95 weight % and 5-50 weight % are preferably 85-95 weight % and 5-15 weight % especially.In addition, if polyoxyalkylene (b) is too much, the tensile strength of curing rubber, physical property such as unit elongation variation sometimes when cutting off.In addition, the a kind of use separately separately of polyoxyalkylene (a) and polyoxyalkylene (b) also can 2 kinds or be used in combination more.
-(B) contain the organopolysiloxane of thiazolinyl-
The known organopolysiloxane that normally uses as the organopolysiloxane that contains thiazolinyl of the present invention (B) component as the basic polymkeric substance of addition curable rubber composition.(B) component is the material that has 2, preferred 2-20, preferred 2-10 the especially siloxane unit by above-mentioned general formula (1) expression in a molecule at least.
To this restriction especially of molecular structure that contains the organopolysiloxane of thiazolinyl, can use have the straight chain shape, the material of siloxane backbone such as ring-type, chain.In general, repeat to constitute, exist the straight chain shape diorganopolysiloxanecompositions of three organic siloxyies basically at molecular chain two ends by two organo-siloxane unit for main chain.
Essential siloxane unit
In general formula (1), R
1The expression carbonatoms is preferably 2-8, is preferably the thiazolinyl of 2-6 especially.Specifically, for example, can enumerate vinyl, allyl group, propenyl, pseudoallyl, butenyl etc., owing to be easy to synthesize, so preferred vinyl.
R
2Identical or different, the common carbonatoms of expression is 1-10, is preferably 1 valency alkyl 1-6, that do not have aliphatics unsaturated link(age), non-replacement or replacement.As using R
21 valency alkyl of expression for example, can be enumerated alkyl such as methyl, ethyl, propyl group, sec.-propyl, butyl, isobutyl-, the tertiary butyl, amyl group, hexyl, cyclohexyl, octyl group; Aryl such as phenyl, tolyl, xylyl; Aralkyl such as benzyl, styroyl; 3,3, the 1 valency alkyl that 3-trifluoro propyl, chloro methyl, chlorophenyl etc. replace with halogen or cyano group etc. preferably can be enumerated methyl, phenyl.
In addition, because good, so (that is, comprise R with whole organic groups of Siliciumatom bonded in (B) component with intermiscibility as the polyoxyalkylene of (A) component
1, R
2With the summation of 1 valency alkyl of non-replacement of Siliciumatom bonded or replacement) 10-50mol%, preferred 10-40mol% be that phenyl is necessary.Under the situation of the not enough 10mol% of this phenyl content, be difficult to mix with polyoxyalkylene, surpassing under the situation of 50mol%, quantitatively synthetic very difficult with high yield.From the above point of view, by R in the general formula (1)
21 valency alkyl of expression except with Siliciumatom bonded phenyl, all is methyl especially preferably.
In general formula (1), a is 1 or 2, and b is the integer of 0-2, and still, a+b is the integer of 1-3.Since synthetic easily, so a is preferably 1.Because a+b can be any value of 1,2 and 3, the siloxane unit that contains this thiazolinyl can be for 1 yuan of functional group's property siloxane unit being positioned at molecule chain end, be positioned at 2 yuan of functional group's property siloxane units of the non-end of molecular chain and any one unit that is positioned at 3 yuan of functional group's property siloxane units of branch-like structure.
As the object lesson of the siloxane unit of representing with above-mentioned general formula (1), can enumerate (CH
2=CH) SiO
3/2, (CH
2=CH)
2SiO
2/2, (CH
2=CH) (CH
3) SiO
2/2, (CH
2=CH) (C
6H
5) SiO
2/2, (CH
2=CH)
2(CH
3) SiO
1/2, (CH
2=CH) (CH
3)
2SiO
1/2, (CH
2=CH) (CH
3) (C
6H
5) SiO
1/2, (CH
2=CH) (C
6H
5)
2SiO
1/2, (CH
2=CH)
2(C
6H
5) SiO
1/2Deng.
This siloxane unit can a kind uses separately, also can 2 kinds or be used in combination more.
Other siloxane unit
In addition, as being present in siloxane unit in the organopolysiloxane molecule that contains thiazolinyl, except the above-mentioned siloxane unit that contains thiazolinyl, for example, can enumerate (CH
3)
3SiO
1/2, (CH
3)
2(C
6H
5) SiO
1/2, (CH
3) (C
6H
5)
2SiO
1/2, (C
6H
5)
3SiO
1/2, (CH
3)
2SiO
2/2, (CH
3) (C
6H
5) SiO
2/2, (C
6H
5)
2SiO
2/2, (CH
3) SiO
3/2, (C
6H
5) SiO
3/2, SiO
4/2Deng.
As in this siloxane unit with Siliciumatom bonded organic group, for example, can enumerate, with R
2Exemplify, do not have 1 valency alkyl of the aliphatics unsaturated link(age), identical or different, non-replacements or replacement etc.
This siloxane unit can a kind uses separately, also can 2 kinds or be used in combination more.
(B) component gives an example
As the organopolysiloxane that contains thiazolinyl of (B) component, for example, can enumerate
(in the formula, m and the n 1-1 that respectively does for oneself, 500, be preferably the integer of 5-500) etc.
Organopolysiloxane molecule about (B) component
There is no particular limitation, is preferably 10-3 to the polymerization degree (that is, the Siliciumatom number in the molecule) as the organopolysiloxane of (B) component, and 000,50-2 more preferably, 000, be preferably 50-1 especially, 000.If this polymerization degree satisfies 10-3,000 scope, the physical strength of curing rubber (below, also abbreviate " cured article " as) is enough, becomes excellent aspect operability.
(B) component is generally 50-100 25 ℃ viscosity, and 000mPas is preferably 100-50, and 000mPas is preferably 500-10,000mPas especially.In addition, (B) component can a kind uses separately, also can 2 kinds or be used in combination more.
With respect to (A) component of 100 weight parts, (B) combined amount of component is generally the 20-200 weight part, is preferably the 20-150 weight part.Under the situation of these combined amount less than 20 weight parts, the problem that discovery exists curing rubber tackiness (viscosity) and unreacted polymer oil to ooze is surpassing under the situation of 200 weight parts, and the resistance value of curing rubber uprises.
-(C) organic hydride diene polysiloxane-
(C) component organic hydride diene polysiloxane of Shi Yonging and (A) component and (B) component reaction and use in the present invention as linking agent.This organic hydride diene polysiloxane had by the forming of an above-mentioned average group accepted way of doing sth (2) expression, in molecule, contain with Siliciumatom bonded hydrogen atom (that is SiH yl) and with Siliciumatom bonded phenyl.
In general formula (2), R
3Represent phenyl as mentioned above, R
4Represent except that phenyl, that do not have the aliphatics unsaturated link(age), non-replacement or replacement, carbonatoms is 1-10 usually, is preferably the 1 valency alkyl of 1-6.As by R
4The non-replacement of expression or 1 valency alkyl of replacement, for example, can enumerate alkyl, cyano ethyl, chloro methyl, 3 such as methyl, ethyl, propyl group, sec.-propyl, butyl, isobutyl-, the tertiary butyl, amyl group, hexyl, cyclohexyl, octyl group, 3, the alkyl that cyano group such as 3-trifluoro propyl replace or halogen replaces, be preferably methyl, ethyl, propyl group, 3,3, the 3-trifluoro propyl.
In addition because better with the intermiscibility of the polyoxyalkylene of (A) component, so (C) in the component content of phenyl preferably account in (C) component and the whole organic groups of Siliciumatom bonded (that is R,
3And R
4Summation) 10mol% or more than, more preferably 10-70mol%, preferred especially 15-70mol%.
In general formula (2), c is the number of 0＜c≤2, and d is the number of 0＜d≤1, and e is the number of 0≤e＜2, and still, c+d+e is the number of 0.7＜c+d+e≤3.Preferred c is the number of 0.07-2, and d is the number of 0.001-1, and e is the number of 0-1.8, and still, c+d+e is the number of 0.8-3.0.More preferably c is the number of 0.1-2, and d is the number of 0.01-1, and e is the number of 0-1.6, and still, c+d+e is the number of 1-2.5.
In a molecule contained and Siliciumatom bonded hydrogen atom be necessary for 2 or more than, be generally 2-300, be preferably 3 or more than, be preferably 3-200 especially.These and Siliciumatom bonded hydrogen atom can be arranged in arbitrary position of molecule chain end and the non-end of molecular chain, also can be positioned at above two kinds of positions simultaneously.The molecular structure of this organic hydride diene polysiloxane is not limited especially, can be any straight chain shape, ring-type, branch-like, structure such as three-dimensional netted.
The polymerization degree (that is, the Siliciumatom number in the molecule) as the organic hydride diene polysiloxane of (C) component is generally 2-1,000, is preferably 3-300, more preferably 4-150.In addition, this organic hydride diene polysiloxane is generally 0.1-100 25 ℃ viscosity, 000mPas, and 0.5-5 more preferably, 000mPas is a fluent meterial in the time of 25 ℃.
Organic hydride diene polysiloxane as (C) component, specifically, for example, can enumerate 1,1,3,3-tetraphenyl sily oxide, 1,1-dimethyl-3,3-phenylbenzene sily oxide, 1,3-dimethyl-1,3-phenylbenzene sily oxide, hydrogenated methyl diene siloxanes diphenyl siloxane cyclocopolymer, hydrogenated methyl diene siloxanes methylphenyl siloxane cyclocopolymer, hydrogenated methyl diene siloxanes dimethyl siloxane diphenyl siloxane cyclocopolymer, two ends are by the hydrogenated methyl diene siloxanes diphenyl siloxane multipolymer of trimethylsiloxy sealing, two ends are by the hydrogenated methyl diene siloxanes methylphenyl siloxane multipolymer of trimethylsiloxy sealing, two ends are by the dimethyl siloxane hydrogenated methyl diene siloxanes diphenyl siloxane multipolymer of trimethylsiloxy sealing, two ends are by the dimethyl siloxane hydrogenated methyl diene siloxanes methylphenyl siloxane multipolymer of trimethylsiloxy sealing, two ends are by the dimethyl siloxane diphenyl siloxane multipolymer of dimethyl hydrogenation diene siloxy-sealing, two ends are by the dimethyl siloxane methylphenyl siloxane multipolymer of dimethyl hydrogenation diene siloxy-sealing, two ends are by the dimethyl siloxane hydrogenated methyl diene siloxanes diphenyl siloxane multipolymer of dimethyl hydrogenation diene siloxy-sealing, two ends are by the dimethyl siloxane hydrogenated methyl diene siloxanes methylphenyl siloxane multipolymer of dimethyl hydrogenation diene siloxy-sealing, by (CH
3)
2HSiO
1/2Unit, SiO
4/2Unit and (C
6H
5)
3SiO
1/2The multipolymer that the unit forms, by (CH
3)
2HSiO
1/2Unit, SiO
4/2Unit and (C
6H
5) SiO
3/2The multipolymer that the unit forms etc.These compositions can a kind use separately, also can 2 kinds or be used in combination more.
(C) combined amount of component for make with respect to (A) component and (B) in (C) component of the contained thiazolinyl of component contained mol ratio with Siliciumatom bonded hydrogen atom be that the amount of 0.1-3.0 is necessary, be preferably and make it become the amount of 0.5-2.0.Under the situation of this mol ratio less than 0.1, cross-linking density step-down, the poor heat resistance of curing rubber.Surpass under 3.0 the situation in this mol ratio, can produce the problem that causes foaming by dehydrogenation reaction, the poor heat resistance of curing rubber.
-(D) platinum group catalyst-
Platinum group catalyst as (D) of the present invention component is the catalyzer with addition reaction (the Ha イ De ロ サ イ レ-シ ヨ Application) effect that promotes above-mentioned (A)-(C) component, can be to well known to a person skilled in the art catalyzer.
As this platinum group catalyst, for example, platinum, platinum series compound etc. are arranged, as object lesson, can enumerate the coordination compound etc. of pure modifier, Platinic chloride and alkene, aldehyde, vinylsiloxane, the alkynol class etc. of platinum black, Platinic chloride, Platinic chloride.
(D) combined amount of component is a significant quantity, can increase and decrease according to desired curing speed.Usually, represent that (D) relative (A) component of the platinum metal ingredient in the component is preferably 0.1-1000ppm, more preferably 1-200ppm with weight basis.(D) component can a kind of independent use, also can 2 kinds or be used in combination more.
-(E) the ionic conductivity imparting agent-
Ionic conductivity imparting agent as the present invention (E) component is the material that is used to give gained curing rubber ionic conductivity.This ionic conductivity imparting agent is an inorganic metal salt, for example, can enumerate an alkali metal salts such as lithium, sodium, potassium; The salt of alkaline-earth metal such as calcium, barium etc.As these object lesson, can enumerate LiClO
4, LiCF
3SO
3, LiN (CF
3SO
2)
2, LiAsF
6, LiCl, NaSCN, KSCN, NaCl, an alkali metal salts such as NaI, KI; Ca (ClO
4)
2, Ba (ClO
4)
2Deng alkali earth metal salt etc.Wherein, good because the resistance value of gained curing rubber is low with the solubleness of other components, so preferred LiClO
4, LiCF
3SO
3, LiN (CF
3SO
2)
2, LiAsF
6, LiCl, preferred especially LiCF
3SO
3, LiN (CF
3SO
2)
2
(A) component of relative 100 weight parts, (E) combined amount of component is preferably the 1-10 weight part for the 0.5-10 weight part is necessary.Under the situation of this combined amount less than 0.5 weight part, can not get target value is 1 * 10
5-1 * 10
7Resistance value about Ω.Surpass under the situation of 10 weight parts in this combined amount, aspect cost, just become problem.
In addition, (E) component can use with its original state, also can be dissolved in advance as in the polyoxyalkylene polymers of (A) component and use.In addition, (E) component can a kind of independent use, also can 2 kinds or be used in combination more.
-other any component-
As required, in the scope of not damaging the object of the invention, can in above-mentioned (A)-(E) component, add following any component.As any component, can enumerate for example weighting agent, heat-resisting toughener, reaction control agent etc.These can independent separately a kind of use, also can 2 kinds or be used in combination more.
Weighting agent
As weighting agent, existing is the material that usually uses in rubber composition, for example, can use atomizing silica, crystallinity silicon-dioxide, settleability silicon-dioxide, silicon-dioxide that hydrophobization handles etc. is carried out on the surface.Because atomizing silica and the settleability silicon-dioxide property strengthened is good, preferred BET specific surface area is 50-500m
2/ g is preferably 100-400m especially
2/ g.Object lesson as above-mentioned weighting agent, represent with trade(brand)name, can enumerate Aerosil 130,200,300 (Japanese ア エ ロ ジ Le societies, Degussa society system), CabosilMS-5, MS-7 (Cabot society system) RheorosilQS-102,103 (moral mountain Cao Da society systems), NipsilLP wetting ability silicon-dioxide such as (Japanese シ リ カ systems); AerosilR-812, R-812S, R-972, R-974 (Degussa society system), RheorosilMT-10 (moral mountain Cao Da society system), NipsilSS series hydrophobic silicas such as (Japanese シ リ カ systems); Crystallite, Minusil, crystallinity silicon-dioxide such as Imisil etc.
(A) component of relative 100 weight parts, the combined amount of above-mentioned weighting agent can mix 300 weight parts or following (that is, the 0-300 weight part), preferred 5-300 weight part, more preferably 10-200 weight part.
The thermotolerance toughener
As the thermotolerance toughener, for example, can use cerium oxide, cerous hydroxide, ferric oxide (iron oxide red), titanium oxide etc.
(A) component of relative 100 weight parts, the combined amount of above-mentioned thermotolerance toughener is preferably the 0-30 weight part, more preferably the 1-30 weight part.
The reaction control agent
When being necessary to adjust the set time of solidifying the present composition, can also add the reaction control agent.As this reaction control agent, for example, can enumerate the organopolysiloxane that vinyl cyclotetrasiloxane etc. contains vinyl; Triallyl isocyanurate, alkyl maleic acid ester, alkynol class and silane thereof, silicone-modified thing; Hydrogen peroxide; Tetramethyl Ethylene Diamine; Benzotriazole; Their mixture etc.
-other-
Addition curable rubber combination of the present invention preferably is liquid material in the time of 25 ℃.
[ionic conductivity rubber coated pressure bowl]
The rubber combination of the invention described above is the composition that uses with material as the roller in electro photography image processing system etc.Specifically, for example, can enumerate charged roller, development roller, the toner supply roller around the photoreceptor in electro photography printer, duplicating machine, the facsimile recorder etc., transcribe roller etc.As this roller, for example, can enumerate the ionic conductivity rubber coated pressure bowl of the ionic conductivity rubber layer that has core and form by the cured article that covers the above-mentioned rubber combination around the core.The manufacture method of such ionic conductivity rubber coated pressure bowl is known, for example, and by following operation manufacturing.In addition, here in example the liquid addition curable rubber combination to optimal way describe.
First-selection, the amount of utilizing the static(al) mixing tank to mix the each several part defined of 2 component-type rubber combinations, perhaps, thereby by using motorized agitator to utilize the each component preparating mixture of spiral rotation rubber blend composition.On the other hand, will implement metal core that bottoming handles in advance rests on and is used in the mould that roller is shaped.Then, in this mould, inject the compound of above-mentioned preparation.Then, the rubber combination that injects by heating makes it to solidify, after the periphery of metal core forms rubber layer, with the rubber coated pressure bowl demoulding.Further, as required, can also be that coating agent, urethane are that coating agent, polyamide-based coating agent, aminosilane are coating agent such as coating agent by coating fluorine on this rubber layer, form the protective layer that forms by this coating agent.
In addition, as other manufacture method, can enumerate following method.First-selection, the amount of utilizing the static(al) mixing tank to mix the each several part defined of 2 component-type rubber combinations, perhaps, thereby by using motorized agitator to utilize the each component preparating mixture of spiral rotation hybrid resin rubber combination.On the other hand, will implement metal core that bottoming handles in advance rests on and is used in the mould that roller is shaped.Then, in this mould, inject the compound of above-mentioned preparation.Then, the rubber combination that injects by heating makes it to solidify, and forms rubber layer in the periphery of metal core, after the rubber coated pressure bowl demoulding, grinds the surface of this rubber coated pressure bowl.Further, as required, can also be that coating agent, urethane are that coating agent, polyamide-based coating agent, aminosilane are coating agent such as coating agent by coating fluorine on this rubber layer, form the protective layer that forms by this coating agent.
The metal core that in the manufacturing of rubber coated pressure bowl of the present invention, uses, for example, can adopt iron, aluminium, stainless steel etc. any one as material.In addition, the metal core that can also use prior bottoming to handle.
[embodiment]
Below, utilize embodiment that the present invention is specifically described, still, the present invention is not limited to these embodiment.In addition, in an embodiment, be meant " (C) in the component contained and Siliciumatom bonded hydrogen atom with respect to (A) component and (B) mol ratio of contained thiazolinyl in the component " as " mol ratio of SiH/ thiazolinyl ".Also have, Ph represents phenyl.
-embodiment 1-
With 100 weight parts, two ends about 7,200), the following formula of 20 weight parts (3) by the polyoxypropylene of allyl group sealing (number-average molecular weight:
(phenyl contains ratio to two ends of expression: 40mol%), the following formula (4) of 10.5 weight parts by the polysiloxane that contains phenyl of vinyl-dimethyl base siloxy-sealing
Viscosity is about the hydrogenated methyl diene siloxanes that the contains phenyl (mol ratio of SiH/ thiazolinyl: 1.5mol/mol), the 1-ethynyl-1-hexalin of the conduct of 0.6 weight part reaction control agent mixes of 20mPas during 25 ℃ of expression.Then, relative (A) component adds 100ppm (is benchmark with weight) and as the platinum vinylsiloxane complex compound of platinum composition, is fully mixed to homogeneous in as above gained mixture.Then, in as above gained mixture, add the LiN (CF of 2 weight parts
3SO
2)
2, 15 weight parts the titan oxide particles as the thermotolerance toughener, thorough mixing, preparation obtains liquid rubber composition 1.
-embodiment 2-
In embodiment 1, (phenyl contains ratio: combined amount 40mol%) changes into 50 weight parts polysiloxane that contains phenyl that two ends of above-mentioned except making (3) expression are sealed by vinyl-dimethyl base siloxy-, and operation preparation similarly obtains liquid rubber composition 2.
-embodiment 3-
With 100 weight parts, two ends about 7,200), the following formula of 20 weight parts (5) by the polyoxypropylene of allyl group sealing (number-average molecular weight:
(phenyl contains ratio to two ends of expression: 10mol%), viscosity is about the hydrogenated methyl diene polysiloxane that the contains phenyl (mol ratio of SiH/ thiazolinyl: 1.2mol/mol), the 1-ethynyl-1-hexalin of the conduct reaction control agent of 0.6 weight part mixes of 20mPas 25 ℃ of the above-mentioned formula of 6.5 weight parts (4) expression times by the polysiloxane that contains phenyl of vinyl-dimethyl base siloxy-sealing.Then, relative (A) component adds 100mm (is benchmark with weight) and as the platinum vinylsiloxane complex compound of platinum composition, is fully mixed to homogeneous in as above gained mixture.Then, in as above gained mixture, add the LiN (CF of 0.6 weight part
3SO
2)
2, 15 weight parts the titan oxide particles as the thermotolerance toughener, thorough mixing, preparation obtains liquid rubber composition 3.
-embodiment 4-
In embodiment 3, (phenyl contains ratio: combined amount 10mol%) changes into 50 weight parts polysiloxane that contains phenyl that two ends of above-mentioned except making (5) expression are sealed by vinyl-dimethyl base siloxy-, operation similarly, preparation obtains liquid rubber composition 4.
[evaluation method]
1-4 injects mould separately with these liquid rubber compositions, with this mold heated to 120 ℃, keeps this temperature 10 minutes, then, with its cure under pressure, produces the sheet curing rubber experiment slice 1-4 of thick 6mm.According to following mensuration benchmark, these experiment slices are measured surface viscosity, oozing property of oil, hardness and resistance value.The results are shown in Table 1 for it.
[measuring method]
1. surface viscosity
By the surface of finger contact curing rubber experiment slice, confirm whether to have viscosity.
2. oozing property of oil
Whether each curing rubber experiment slice after room temperature leaves standstill after solidifying, confirms to exist the oil on surface to ooze by naked eyes at 24 o'clock.
3. hardness
Overlapping 2 experiment slices (sheet of thick 6mm) use ア ス カ-C type hardness tester meter to measure.
4. resistance value
To between metal shaft and battery lead plate, insert experiment slice (sheet of thick 6mm).On experiment slice, hang up in the 1kg heavy burden, between metal shaft and battery lead plate, add the volts DS of 10V, 100V, 500V, measure resistance value.
-comparative example 1-
In embodiment 1, (phenyl contains ratio: 40mol%), similarly operate, preparation obtains liquid rubber composition C1 to the polysiloxane that contains phenyl that is sealed by vinyl-dimethyl base siloxy-except two ends that do not add above-mentioned (3) expression.
-comparative example 2-
In embodiment 1, (phenyl contains ratio: combined amount 40mol%) changes into 10 weight parts polysiloxane that contains phenyl that two ends of above-mentioned except making (3) expression are sealed by vinyl-dimethyl base siloxy-, operation similarly, preparation obtains liquid rubber composition C2.
-comparative example 3-
In embodiment 3, (phenyl contains ratio: combined amount 10mol%) changes into 10 weight parts polysiloxane that contains phenyl that two ends of above-mentioned except making (5) expression are sealed by vinyl-dimethyl base siloxy-, operation similarly, preparation obtains liquid rubber composition C3.
[evaluation method]
C1-C3 injects mould separately with these liquid rubber compositions, with this mold heated to 120 ℃, keeps this temperature 10 minutes, then, with its cure under pressure, makes the sheet curing rubber experiment slice C1-C3 of thick 6mm.According to following mensuration benchmark, these experiment slices are measured surface viscosity, oozing property of oil, hardness and resistance value.The results are shown in Table 1 for it.
Physical property of (table 1) rubber combination and electrical characteristic
[table 1]
| Embodiment 1 (experiment slice 1) | Embodiment 2 (experiment slice 2) | Embodiment 3 (experiment slice 3) | Embodiment 4 (experiment slice 4) | Comparative example 1 (experiment slice C1) | Comparative example 2 (experiment slice C2) | Comparative example 3 (experiment slice C3) | |
| Surface viscosity | Do not have | Do not have | Do not have | Do not have | Have | Have | Have |
| Oozing property of oil | Do not have | Do not have | Do not have | Do not have | Have | Have | Have |
| Hardness (ア ス カ-C type) | ????43 | ????43 | ????27 | ????27 | ????42 | ????42 | ????26 |
| Resistance during impressed voltage 10V (Ω) | ??4.4×10 7 | ?4.5×10 7 | ??1.7×10 7 | ??1.8×10 7 | ??2.7×10 7 | ??8.4×10 7 | ??5.3×10 7 |
| Resistance during impressed voltage 100V (Ω) | ??4.0×10 7 | ?4.0×10 7 | ??12×10 7 | ??12×10 7 | ??2.0×10 7 | ??3.6×10 7 | ??2.5×10 7 |
| Resistance during impressed voltage 500V (Ω) | ??4.4×10 7 | ?4.4×10 7 | ??1.3×10 7 | ??1.3×10 7 | ??2.7×10 7 | ??2.6×10 7 | ??2.7×10 7 |
-embodiment 5-
With the polyoxypropylene (number-average molecular weight: about 7,200) of 100 weight parts, two ends by the allyl group sealing, 5 weight parts, two ends are by the polyoxypropylene (number-average molecular weight: about 480) of allyl group sealing, (phenyl contains ratio to the polysiloxane that contains phenyl that two ends of the above-mentioned formula of 50 weight parts (3) expression are sealed by vinyl-dimethyl base siloxy-: 40mol%), 12.6 viscosity is about the hydrogenated methyl diene polysiloxane (mol ratio of SiH/ thiazolinyl: 1.3mol/mol) that contains phenyl of 20mPas during 25 ℃ of the above-mentioned formula of weight part (4) expression, 0.6 the 1-ethynyl-1-hexalin of the conduct of weight part reaction control agent mixes.Then, relative (A) component adds 100ppm (is benchmark with weight) and as the platinum vinylsiloxane complex compound of platinum composition, is fully mixed to homogeneous in as above gained mixture.Further, in as above gained mixture, add the LiN (CF of 2 weight parts
3SO
2)
2, thorough mixing, preparation obtains liquid rubber composition 5.
-embodiment 6-
In embodiment 5, except make two ends by the polyoxypropylene of allyl group sealing (number-average molecular weight: combined amount about 480) changes into 10 weight parts, operation similarly, preparation obtains liquid rubber composition 6.
[evaluation method]
This liquid rubber composition 5 and 6 is injected mould separately,, kept this temperature 10 minutes, then,, make the sheet curing rubber experiment slice 5 and 6 of thick 6mm its cure under pressure with this mold heated to 120 ℃.To these experiment slices with the energising of the voltage of 100V, under this voltage, (0 hour) when measuring the energising beginning respectively, through the resistance value after 0.5 hour, 1 hour, 2 hours.The results are shown in Table 2 for it.
(table 2) resistance value (Ω) is over time when energising voltage 100V
[table 2]
| 0 hour | 0.5 hour | 1 hour | 2 hours | |
| Embodiment 5 (experiment slice 5) | ?3.5×10 7 | ??3.7×10 7 | ?4.1×10 7 | ??4.1×10 7 |
| Embodiment 6 (experiment slice 6) | ?4.4×10 7 | ??4.7×10 7 | ?4.8×10 7 | ??4.8×10 7 |
＜estimate
In the comparative example 1 of two ends that does not mix as (B) component, find to solidify the rubber combination of gained and the curing rubber that obtains exists surface viscosity and oozing property of oil by the polysiloxane that contains phenyl of vinyl-dimethyl base siloxy-sealing.In making the comparative example 2 and 3 that is in by the combined amount of the polysiloxane that contains phenyl of vinyl-dimethyl base siloxy-sealing as two ends of (B) component as 10 weight parts beyond the specialized range, the curing rubber of not only finding to solidify the gained rubber combination and obtaining exists surface viscosity and perviousness, and along with the variation of impressed voltage, resistance value is deficient in stability also.
[effect of invention]
The liquid addition curable rubber composition of the application of the invention does not have adherence (viscosity) and oozing property of oil on the curing rubber surface after being heating and curing, form the stable composition of resistance value with respect to the variation of applied voltage.
In addition, be 5 using the number-average molecular weight that contains the 50-98 % by weight as the polyoxyalkylene that has at least 2 thiazolinyls in the molecule of (A) component, 000 or the embodiment of the resin combination of the number-average molecular weight 500 of the above polyoxyalkylene with thiazolinyl and 2-50 % by weight or the following polyoxyalkylene with thiazolinyl in, can also suppress resistance value with respect to the energising voltage rising in time of gained curing rubber.
In addition, use said composition, can also make the ionic conductivity rubber coated pressure bowl of physical characteristic and electrical characteristics excellence.
Claims (9)
1. roller addition curable rubber combination, it contains
(A) in a molecule, contain the polyoxyalkylene of 2 thiazolinyls at least: 100 weight parts
(B) in a molecule, have 2 at least with general formula (1):
R
1 aR
2 bSiO
(4-a-b)/2??(1)
(in the formula, R
1The expression thiazolinyl, R
2Represent identical or different, that do not have the aliphatics unsaturated link(age), non-replacement or replacement 1 valency alkyl, a is 1 or 2, b is the integer of 0-2, wherein, a+b is the integer of 1-3) expression organopolysiloxane siloxane unit, that contain thiazolinyl: the 20-200 weight part, wherein this organopolysiloxane contain account for the whole organic group 10-50mol% of Siliciumatom bonded with Siliciumatom bonded phenyl
(C) with an average group accepted way of doing sth (2):
R
3 cH
dR
4 eSiO
(4-c-d-e)/2??(2)
(in the formula, R
3The expression phenyl, R
4Represent except that phenyl, do not have the aliphatics unsaturated link(age), 1 valency alkyl of non-replacement or replacement, c is the number of 0＜c≤2, d is the number of 0＜d≤1, e is the number of 0≤e＜2, but, c+d+e is the number of 0.7＜c+d+e≤3) expression, at least contain 2 organic hydride diene polysiloxane with Siliciumatom bonded hydrogen atom in a molecule: its content is for making in (C) component that contained and Siliciumatom bonded hydrogen atom are the amount of 0.1-3.0 with respect to the mol ratio of contained thiazolinyl at (A) and (B)
(D) platinum group catalyst: significant quantity
And
(E) ionic conductivity imparting agent: 0.5-10 weight part.
2. rubber combination as claimed in claim 1, wherein to contain the number-average molecular weight of 50-98 weight % be 5,000 or the above polyoxyalkylene that contains thiazolinyl and the number-average molecular weight 500 of 2-50 weight % or the following polyoxyalkylene that contains thiazolinyl to (A) component.
3. rubber combination as claimed in claim 1 or 2, wherein the thiazolinyl in (A) component is present in two ends of polyoxyalkylene molecule at least.
4. as any described rubber combination of claim 1-3, wherein said polyoxyalkylene is a polyoxypropylene.
5. as any described rubber combination of claim 1-4, wherein in described general formula (1), R
2The expression 1 valency alkyl except with Siliciumatom bonded phenyl all be methyl.
6. as any described rubber combination of claim 1-5, wherein in (C) component the content of phenyl account in (C) component with the 10mol% of the whole organic groups of Siliciumatom bonded or more than.
7. as any described rubber combination of claim 1-6, wherein (E) ionic conductivity imparting agent contains LiCF
3SO
3And/or LiN (CF
3SO
2)
2
8. ionic conductivity rubber coated pressure bowl, it has core and covers the ionic conductivity rubber layer that the cured article by any described rubber combination of claim 1-7 around this core forms.
9. rubber coated pressure bowl as claimed in claim 8 wherein also has the protective layer that is formed by coating in the periphery of described ionic conductivity rubber layer.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP128715/03 | 2003-05-07 | ||
| JP128715/2003 | 2003-05-07 | ||
| JP2003128715A JP3914511B2 (en) | 2003-05-07 | 2003-05-07 | Rubber composition for roll and ion conductive rubber roll using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1572835A true CN1572835A (en) | 2005-02-02 |
| CN100415832C CN100415832C (en) | 2008-09-03 |
Family
ID=33504758
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100451892A Expired - Fee Related CN100415832C (en) | 2003-05-07 | 2004-04-30 | Rubber composition for roller and ionic conductive rubber roller using the composition |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP3914511B2 (en) |
| KR (1) | KR100989275B1 (en) |
| CN (1) | CN100415832C (en) |
| TW (1) | TW200502323A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821309B (en) * | 2005-02-15 | 2011-06-08 | 信越化学工业株式会社 | Insulation silicon rubber compound |
| CN102464887A (en) * | 2010-11-18 | 2012-05-23 | 达兴材料股份有限公司 | Hardenable siloxane resin composition for light emitting diode element |
| TWI398487B (en) * | 2005-12-06 | 2013-06-11 | Shinetsu Chemical Co | A polysiloxane composition and a hardened product thereof |
| TWI408175B (en) * | 2005-03-23 | 2013-09-11 | Shinetsu Chemical Co | Fixed roller or fixed belt with insulating silicone rubber composition, and fixed roller and fixed belt |
| CN103421323A (en) * | 2012-05-22 | 2013-12-04 | 信越化学工业株式会社 | Antistatic silicone rubber composition and a silicone rubber antistatic inhibiting yellowing of the cured method |
| TWI653296B (en) | 2018-03-23 | 2019-03-11 | 英濟股份有限公司 | Liquid silicone rubber composition, method for manufacturing thereof, and oral isolator manufactured thereby |
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| JP5186754B2 (en) * | 2006-11-14 | 2013-04-24 | トヨタ自動車株式会社 | Fuel cell |
| JP5082467B2 (en) | 2007-01-29 | 2012-11-28 | トヨタ自動車株式会社 | Fuel cell and separator constituting fuel cell |
| JP5758845B2 (en) * | 2012-05-23 | 2015-08-05 | 信越化学工業株式会社 | Silicone rubber composition |
| JP5468712B1 (en) * | 2012-11-05 | 2014-04-09 | モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 | Thermosetting silicone rubber composition |
| WO2014069622A1 (en) * | 2012-11-05 | 2014-05-08 | モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 | Thermosetting silicone rubber composition |
| JP5935749B2 (en) * | 2013-04-25 | 2016-06-15 | 信越化学工業株式会社 | Addition-curing rubber composition for roll, ion conductive rubber roll, and electrophotographic image forming apparatus |
| JP6773569B2 (en) * | 2016-02-15 | 2020-10-21 | 三洋化成工業株式会社 | Antistatic silicone resin composition |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3543868B2 (en) * | 1994-03-07 | 2004-07-21 | 鐘淵化学工業株式会社 | Roller compositions and rollers therefrom |
| JP3518895B2 (en) * | 1994-07-28 | 2004-04-12 | 鐘淵化学工業株式会社 | Curable conductive composition |
| JPH09292754A (en) * | 1996-04-26 | 1997-11-11 | Kanegafuchi Chem Ind Co Ltd | Roller |
| JP3493901B2 (en) * | 1996-06-17 | 2004-02-03 | 鐘淵化学工業株式会社 | Developing roller |
| JP3605976B2 (en) * | 1996-12-26 | 2004-12-22 | 株式会社カネカ | Developing roller |
| JP3794111B2 (en) * | 1997-07-01 | 2006-07-05 | 株式会社カネカ | Developing roller |
| JP2000309709A (en) * | 1999-04-27 | 2000-11-07 | Kanegafuchi Chem Ind Co Ltd | Curable conductive composition and conductive rubber roller made by using it |
| JP2001323164A (en) * | 2000-05-12 | 2001-11-20 | Kanegafuchi Chem Ind Co Ltd | Curable composition for roller and rubber roller made therefrom |
| CN1280351C (en) * | 2000-12-07 | 2006-10-18 | 钟渊化学工业株式会社 | Semiconductive resion composition and semiconductive member |
| JP3874072B2 (en) * | 2001-04-05 | 2007-01-31 | 信越化学工業株式会社 | Silicone rubber composition for fixing roll and fixing roll |
| JP2002311685A (en) * | 2001-04-16 | 2002-10-23 | Kanegafuchi Chem Ind Co Ltd | Composition for roller and conductive roller manufactured by using the same |
-
2003
- 2003-05-07 JP JP2003128715A patent/JP3914511B2/en not_active Expired - Fee Related
-
2004
- 2004-04-30 CN CNB2004100451892A patent/CN100415832C/en not_active Expired - Fee Related
- 2004-05-06 KR KR1020040031611A patent/KR100989275B1/en active IP Right Grant
- 2004-05-06 TW TW093112781A patent/TW200502323A/en not_active IP Right Cessation
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821309B (en) * | 2005-02-15 | 2011-06-08 | 信越化学工业株式会社 | Insulation silicon rubber compound |
| TWI408175B (en) * | 2005-03-23 | 2013-09-11 | Shinetsu Chemical Co | Fixed roller or fixed belt with insulating silicone rubber composition, and fixed roller and fixed belt |
| TWI398487B (en) * | 2005-12-06 | 2013-06-11 | Shinetsu Chemical Co | A polysiloxane composition and a hardened product thereof |
| CN102464887A (en) * | 2010-11-18 | 2012-05-23 | 达兴材料股份有限公司 | Hardenable siloxane resin composition for light emitting diode element |
| CN102464887B (en) * | 2010-11-18 | 2013-09-04 | 达兴材料股份有限公司 | Hardenable siloxane resin composition for light emitting diode element |
| CN103421323A (en) * | 2012-05-22 | 2013-12-04 | 信越化学工业株式会社 | Antistatic silicone rubber composition and a silicone rubber antistatic inhibiting yellowing of the cured method |
| CN103421323B (en) * | 2012-05-22 | 2018-01-23 | 信越化学工业株式会社 | The method of the xanthochromia of Antistatic silicone rubber composition and suppression antistatic behaviour silicon rubber solidfied material |
| TWI653296B (en) | 2018-03-23 | 2019-03-11 | 英濟股份有限公司 | Liquid silicone rubber composition, method for manufacturing thereof, and oral isolator manufactured thereby |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2004331786A (en) | 2004-11-25 |
| TWI324624B (en) | 2010-05-11 |
| KR20040095667A (en) | 2004-11-15 |
| KR100989275B1 (en) | 2010-10-20 |
| CN100415832C (en) | 2008-09-03 |
| JP3914511B2 (en) | 2007-05-16 |
| TW200502323A (en) | 2005-01-16 |
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