CN104262797B - A kind of unvulcanized rubber composition - Google Patents
A kind of unvulcanized rubber composition Download PDFInfo
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- CN104262797B CN104262797B CN201410484753.4A CN201410484753A CN104262797B CN 104262797 B CN104262797 B CN 104262797B CN 201410484753 A CN201410484753 A CN 201410484753A CN 104262797 B CN104262797 B CN 104262797B
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
A kind of unvulcanized rubber composition, cleans the organic compound penetrating agent of effect and catalyst thereof and carrier material thereof including rubber, peroxide vulcanizing system, inserts, plasticizer, mould release, detergent, enhancing.This rubber compound can thoroughly clean mould dirt, has good fillibility and ripening rubbery intensity, brittle failure will not occur, fall bits, unfilled corner, and clear mould job safety is convenient.
Description
Technical field
The present invention relates to technical field of electronic encapsulation, especially relate to a kind of clean the unvulcanized of Electronic Packaging mould
Rubber.
Background technology
In Electronic Packaging industry, metal die and epoxy molding plastic are widely used to realize semiconductor die package
The industrialized production of ChipMolding.Metal die be precise construction can close tight multi-cavity position mould by upper and lower mould
Chamber, epoxy molding plastic is the heat-curable compounds using one-component, containing latent curing agent, filler, many
Plant ten Multiple components such as auxiliary agent.
Conventional technique be pre-to (high frequency) thermal softening after epoxy molding plastic pressure injection enter upper and lower mould and close tightly
Die cavity, about 170 DEG C solidification several minutes, die sinking, take out product, complete once " plastic packaging " operation.?
After hundreds of or thousands of times of this plastic packaging work cycle repeatedly, die surface inevitably there occurs pollution.Enter
And outward appearance and the quality of product can be affected.In plastic packaging operation, remove these pollutant with melamine resin and be referred to as " clear
Mould " operation.From the sixties in last century so far, clear mould operation is due to holding time length, cost height, molding die cleaning materials
Brittle failure can occur, to fall bits, unfilled corner etc. bad, easily causes mould damage, become the most always time accidentally
Plastic packaging operation needs the bothersome job of careful operation.
At the end of the nineties, the melamine resin system that a kind of cleaning method using unvulcanized rubber composition becomes traditional is clear
The contenders of washing method.Observe die surface dirt analysis find, 1, the dirt of die surface be with
The increase of plastic packaging operations number is thickening, and the thickening speed of dirt is not homogeneous constant.2, cavity surface
Dirt thickness is not equally distributed.With Temperature Distribution and epoxy molding plastic in the flowing velocity of mold cavity surface
Etc. relevant, region that Temperature Distribution is high and epoxy molding plastic are at the slow region dirt of the flowing velocity of mold cavity surface
Thicker.
Usually, melamine resin system clean to dirt viscous go out effect be continuous and effective, but melamine resin system is clear
Wash to dirt viscous go out effect less, it appears that be to peel off the most uniformly, need repeated multiple times 10～20
Secondary clear mould operation just can be fully erased.Repeated multiple times clear mould can be close to being substantially removed from dirt.
Use unvulcanized rubber composition cleaning method its that dirt completely glues effect is very big, the most only need honey
Same effect is reached in less than the 1/2 of polyimide resin system cleaning modulus, thus rate of imitating clearly is much higher than melamine resin
System.And need not use lead frame, reduce the cost of clear mould operation；But use half finished rubber group
The cleaning method of compound its to be attached to the meagre dirt in Mold Metal surface viscous go out effect be not continuous and effective
, its effect is more dependent on the formula design of unvulcanized rubber composition.
General thinks, the chemical composition of dirt is relevant with the chemical composition of epoxy molding plastic, is epoxidation
Compound, natural waxes, synthetic wax class, amine (catalyst), fire retardant, filler etc. are attached to the gold of mould
Metal surface, after long high-temperature baking, has the chemical change of dehydration, carbonization, oxidation, be dehydrated,
The degree of oxidation has proportional relation with the time of high-temperature baking.
After the clear mould operation of cleaning method that is repeated multiple times and that examine use unvulcanized rubber composition, thing
Dirt can be divided on Shi and being made up of surface layer and internal layer, surface layer dirt is thicker, and internal layer dirt is the thinnest.(its
The bright and clean degree on the most corresponding encapsulating products epoxy molding plastic surface, the thicker then product epoxy of surface contaminants on moulds
Moulding compound poor surface finish, gloss need to do clear mould operation when requiring less than regulation.There is the thinnest internal layer dirt
Time product epoxy molding plastic surface smoothness preferable, cleaning completely is good without surface smoothness during dirt.
For using its cleaning to surface layer dirt of cleaning method of unvulcanized rubber composition, " investigation of materials
With application " in December, 2010 volume 4 the 4th phase " for the research of integrated circuit packaging mould cleaning material "
One literary composition provides basic formula and preparation method, comprises rubber, filler, ammoniac compounds, DCP initiation
Agent etc..But the filling capacity of current half finished rubber, intensity, toughness and cleaning performance, still the most very
Good comprehensive coordination.
Summary of the invention
The problems referred to above existed for prior art, the applicant provides a kind of unvulcanized rubber composition.This
Rubber compound can thoroughly clean mould dirt, has good fillibility and ripening rubbery intensity, will not
Brittle failure occurring, falls bits, unfilled corner, clear mould job safety is convenient.
Technical scheme is as follows:
A kind of unvulcanized rubber composition, including rubber, peroxide vulcanizing system, inserts, plasticizer,
Mould release, detergent, enhancing clean the organic compound penetrating agent of effect and catalyst thereof and carrier material thereof.
Described rubber is: butadiene-styrene rubber, butadiene rubber, EP rubbers, ethylene propylene diene rubber, polyurethane rubber,
At least two kinds of acrylate rubber；Its usage amount is described unvulcanized rubber composition total amount
50～80wt%.Described rubber is selected from the combination of unsaturated non-polar rubber with saturated nonpolar rubber.
Described peroxide vulcanizing system is: cumyl peroxide, 2,5 di-t-butyl-2,5-(di-t-butyl mistakes
Oxygen) hexane, di-tert-butyl peroxide, t-butyl perbenzoate, 3,3 pairs of (t-butyl peroxy) ethyl n-butyrate .s,
At least one of tert butyl isopropyl benzene peroxide；Its usage amount is described unvulcanized rubber composition total amount
2～5wt%.
Described inserts is: Pulvis Talci, activated clay, silicon powder, silicon dioxide powder, alumina powder, oxidation
Zinc powder, precipitated calcium carbonate, potter's clay, calcium silicates, calcium aluminate, magnesium carbonate, barium sulfate, titanium dioxide, zinc
At least one of barium white；Its usage amount is the 16～40wt% of described unvulcanized rubber composition total amount.
Described plasticizer is: stearic acid, dodecylic acid, di-n-butyl succinate, dibutyl phthalate, liquid
At least one of paraffin body；Its usage amount is the 0.1～5wt% of described unvulcanized rubber composition total amount.
Described mould release is: bar wax, short chain polyethylene, paraffin, silicone oil at least one；Its usage amount is institute
State the 0.01～5wt% of unvulcanized rubber composition total amount.
Described enhancing is cleaned the organic compound penetrating agent of effect and is included at least one of following raw material:
130～180 DEG C of compounds that dehydration can occur, including following several: (1) alcohol catalysis anhydro compounds:
Normal propyl alcohol, 4-hydroxy-4-methyl-2-pentanone, ethylene glycol；(2) carboxylic acid catalytic dehydration compound: adipic acid,
1,5-pentanedicarboxylic acid.；(3) alcohol amine compound and aldehydes anhydro compounds: ethanolamine, diethanolamine, 2-amino 2-ethyl
1,3-propylene glycol, 2-amino 2-methyl 1-propanol, formaldehyde, propionic aldehyde；Its usage amount is described half finished rubber group
The 0.1～10wt% of compound total amount.
Described detergent is at least one in following raw material: N-methyl is than pyrrolidone, dimethyl sulfoxide, second two
Alcohol ethylether, ethylene glycol monobutyl ether, monoethanolamine, diethanolamine, triethanolamine, diethylenetriamine, 2-
Amino 2 methyl 1-propanol, DAA, isopropylideneacetone, ethyl levulinate, Butyl acetylpropanoate,
Hexachlorethane, 1,1,1 trichloroethane, cumene, diisopropyl benzene, 4-amido amylalcohol, ethylene glycol,
1,5-pentanedicarboxylic acid., Ketocyclopentane, Ketohexamethylene；Five yuan, 6-membered heterocyclic compound and derivant thereof: imidazoles, methyl miaow
Azoles, oxazole, oxazolidine, dimethyl oxazolidine, dioxane, furan, oxolane；Its usage amount is
The 0.1～5wt% of described unvulcanized rubber composition total amount.
Described catalyst is: sulphuric acid, nitric acid, hydrochloric acid, phosphoric acid, ethylsulfonic acid, pyrovinic acid, to toluene sulphur
Acid, boric acid, potassium hydroxide, sodium hydroxide, barium hydroxide, sodium silicate, potassium tert-butoxide, sodium tert-butoxide,
At least one of iodine；Its usage amount is the 0.01～10wt% of described unvulcanized rubber composition total amount.
Described carrier material is: molecular sieve, kieselguhr, natural zeolite, permutite at least one；It makes
Consumption is the 1～10wt% of described unvulcanized rubber composition total amount.
Described compositions also includes viscosifying material, and described thickening material is: chlorosulfonated polyethylene, boric acid, ancient horse
At least one in grand, Colophonium；Its usage amount is the 0.1～5wt% of unvulcanized rubber composition total amount.
The particularly preferably unsaturated non-polar rubber of rubber raw rubber and the combination of saturated nonpolar rubber.Vulcanizing system is examined
Consider the environmental requirement to semiconductor factory, have the sulfur cross-linking system of abnormal flavour than it, select peroxide cure
Agent abnormal smells from the patient can be less.Penetrating agent can occur dehydration at 130～180 DEG C.
The addition of mould release, is to prevent the Mold Metal surface the cleaned bonding to epoxy molding plastic.Though
In epoxy molding plastic, so there is the composition of mould release, but in the case of die surface cleaning, epoxy molding plastic
The component amount of middle mould release is insufficient, has the risk of sticking to mould.It is thus desirable at unvulcanized rubber composition
Thing supplements.
In this unvulcanized rubber composition in order to make reversible reaction toward dehydration direction carry out, need use catalyst with
And the carrier material that rugged catalyst plays a role, such as strong acid, highly basic and special catalyst.
The applicant is it has been observed that the thickness that the speed of growth of surface contaminants on moulds is as dirt increases change
, when dirt thickness to dirtier degree, its speed of growth can accelerate many.Internal layer dirt growth time
Length, thickness are thin；Outer layer dirt grows on the basis of internal layer dirt, and the fast growth time is shorter, thickness
Thicker.Namely it could mean that the dirt being adjacent to metal is high because time length and temperature height are dehydrated degree of oxidation,
And outer layer dewatering dirt degree of oxidation is low.
In unvulcanized rubber composition clear mould operation, triethanolamine that rubber composition contains, diethylenetriamine,
2-(methylamine amino) ethanol, further as N-methyl than pyrrolidone, dimethyl sulfoxide, glycol ethyl ether,
The cooperation of diethyl succinate equal solvent penetrates into die surface, makes dirt swelling, the life that rubber composition contains
Glue and filler and other auxiliary agents, the combination of coordination compound, produce polyreaction ripening in initiator decomposes
The dirt that Cheng Zhonghui bonding is swelling, is taken out of dirt by the rubber of ripening during the demoulding.
Applicants have discovered that, to outer layer dirt use comprise rubber, filler, ammoniac compounds, initiator etc. with
And N-methyl is than pyrrolidone, dimethyl sulfoxide, glycol ethyl ether, monoethanolamine, diethanolamine, three second
Hydramine is effective, but such component coordinate unvulcanized rubber composition its to internal layer dirt clean
Power is weak, and repeated multiple times clear mould also cannot be substantially removed from dirt.And dirt is once a clear mould operation
In be not divided, this dirt will in ensuing plastic packaging operation further long-time high-temperature baking, enter
One step dehydration, oxidation, dirt also can become thicker, more obstinate, naturally in ensuing clear mould operation also
It is to be substantially removed from dirt, finally results in mould yields degradation.Other strengths can only be sought
Method for cleaning.Impact produces and produces higher cost.
In " mold cleaning composition " patent of Nitto Denko Corp (publication number CN101077995A),
Propose to comprise the water of 1～20wt% in mold cleaning composition.For the cleaning completely of dirt, mechanism is managed
Solving, the internal layer dirt that the intervention of water can make dehydration serious is converted into the chemical property of outer layer dirt, thus becomes
Easily it is eliminated.
Although a small amount of water is directly added in unvulcanized rubber composition, the ability removing dirt can increase
By force.But it is inoperative to thoroughly removing dirt, a kind of is probably the infiltration of a small amount of water by outer layer dirt
Barrier and internal layer dirt cannot be applied directly to.Increase the addition of water, 1) can make rubber and filler and
His auxiliary agent, the combination of coordination compound suffer damage, and reduce its strengthening action to rubber, reduce unvulcanized
Rubber composition bonds the effect of dirt in maturing process；2) N-methyl is diluted than pyrrolidone, dimethyl
Sulfoxide, glycol ethyl ether equal solvent concentration, cause it and weaken the swelling action of dirt.Result is: not only
Imitate clearly fruit to decline, and the rubbery intensity of ripening declines to a great extent, and has brittle failure, falls the bad generations such as bits.
The applicant chances in experiment repeatedly, can produce dehydration anti-in indivedual organic chemical reactions equations
Answer, and if its reactant and unvulcanized rubber composition non-contravention, be subject at unvulcanized rubber composition
While thermal polymerization, the chemical reaction of its dehydration has the effect removing internal layer dirt.
The applicant repeatedly it was found that, when unvulcanized rubber composition introduces strong organic of permeability
Compound, the ability removing dirt can strengthen.
The applicant repeatedly it was found that, when unvulcanized rubber composition introduces permeability strong and
130～180 DEG C of temperature conditionss issue the organic compound of biochemical change, and its product is also strong the having of permeability
When machine compound and water, after unvulcanized rubber composition adds these organic compound, half finished rubber group
Compound is removed the ability of outer layer dirt and internal layer dirt and can be strengthened especially.
The applicant repeatedly it was found that, 1) at the unvulcanized rubber composition introducing dehydration design
In thing, imitate clearly the upper reactant introducing dehydration design of fruit and product needs to be strong organic of permeability
Compound.2) in the unvulcanized rubber composition introducing dehydration design, the upper mixing of fruit two kinds is imitated clearly
And above type of dehydration is better than single type dehydration in the ability removing dirt.3) de-in introducing
In the unvulcanized rubber composition of water reaction designing, compared with the effect being directly added into water, half finished rubber group
Compound mobility fillibility is good, and unfilled corner will not occur.The rubber composition intensity of ripening is good, will not occur crisp
Break, fall the bad phenomenon such as wadding.4) organic compound of dehydration design, its reactant and product are in temperature
Spending high areal area and show higher vapour pressure, the dirt removal effect in the region high to Temperature Distribution is more preferable.
There is the clean effect of balance.5) add thickening material, make rubber composition and water suction, the swelling dirt of ripening
Thing caking property improves, and dirt removal effect is more preferable.
Understanding in mechanism is, the organic compound that permeability is strong penetrates readily through the barrier of outer layer dirt and directly makees
Using internal layer dirt, the water produced by thermal response is applied directly to internal layer dirt so that it is water suction, swelling.
Useful the having the technical effect that of the present invention
The reactant of this unvulcanized rubber composition dehydration and the chemical equation of product be:
1, alcohol catalysis dehydration
(1) intramolecular dehydration alkanol is dehydrated under acid catalysis
(2) intramolecular dehydration 4-hydroxy-4-methyl-2-pentanone is heated to about 150 DEG C dehydration lifes under catalysis of iodine
Become strong infiltrative isopropylideneacetone and water.
(3) intermolecular dehydration, heating and acid catalysis alcohol generate ether and water
(4) ethylene glycol generates Isosorbide-5-Nitrae-dioxane and water with sulphuric acid or phosphoric acid heat dehydration altogether
2, carboxylic acid dehydration
Such as adipic acid, 1,5-pentanedicarboxylic acid. heat then strong by the intramolecular mistake carboxylic generation of dehydration simultaneously in the presence of barium hydroxide
The cyclic ketones of cleaning strength and water.
3, alcohol amine compound and aldehydes generate the five-membered heterocycles that cleaning strength is the strongest under catalytic condition
And water, such as following 5 reaction examples have particularly preferred mold wash effect.
Detailed description of the invention
Embodiment 1
In 55 liters of adding pressure type banburies, add 11.0kg ethylene propylene diene rubber, 11.0kg butadiene rubber and 0.5kg
Butadiene-styrene rubber.Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add
10.0kg silicon powder, 6.0kg Pulvis Talci, 2.0kg activated clay, detergent: glycol ethyl ether 0.3kg,
Triethanolamine 0.3kg, plasticizer: dodecylic acid 2.2kg, mould release: bar wax 0.05kg.And it is organic de-
Water compound of reaction penetrating agent: DAA 0.05kg catalyst carrier material: 4A molecular sieve 0.65kg and
The catalyst adsorbed: iodine 0.005kg, banburying of pressurizeing, mixing 10 minutes；Uncap, not discharging, then add
Enter 1.0kg cumyl peroxide, mixing 60 seconds.Discharging.The material mixed is crossed two-roll mill,
By ironed for elastomeric compound roller machine thick to about 10mm.It is cut to wide 15mm, the adhesive tape of long 220mm with bale splitter.
Embodiment 2
In 55 liters of adding pressure type banburies, add 20.0kg ethylene propylene diene rubber and 1.0kg acrylate rubber.
Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg lightweight
Calcium carbonate, 2.0kg potter's clay, 2.0kg Griffith's zinc white., detergent: N-methyl is than pyrrolidone 2.2kg, diethanolamine
0.2kg, plasticizer: di-n-butyl succinate 0.2kg, mould release: short chain polyethylene 2.2kg and organic de-
Water compound of reaction: penetrating agent ethanolamine 0.40kg, natural zeolite 0.40kg and catalyst: sodium silicate 4.5kg
And the formaldehyde 0.10kg of absorption；Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 2.3kg
2,5 di-t-butyl-2,5-(di-t-butyl peroxide) hexane, mixing 60 seconds.Discharging.The most double for the material mixed
Roller mill, by ironed for elastomeric compound roller machine thick to about 10mm.It is cut to wide 15mm, long 220mm with bale splitter
Adhesive tape.
Embodiment 3
In 55 liters of adding pressure type banburies, add 13.6kg butadiene rubber, 11.0kg EP rubbers and thickening thing
Matter: 0.5kg chlorosulfonated polyethylene.Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing
3 minutes；Addition 7.5kg silicon dioxide powder, 1.5kg precipitated calcium carbonate, 0.5kg titanium dioxide, detergent:
Dimethyl sulfoxide 0.015kg, ethylene glycol monobutyl ether 0.015kg, imidazoles 0.015kg, plasticizer: stearic acid 0.2kg,
Mould release: paraffin 0.02kg, bar wax 0.02kg；And penetrating agent: ethanolamine 4.5kg, catalyst carrier material
Material: natural zeolite 4.5kg and the catalyst adsorbed: sodium hydroxide 0.01kg and formaldehyde 0.4kg, adds densification
Refining, mixing 10 minutes；Uncap, not discharging, add 0.90kg 3,3 pairs of (t-butyl peroxy) butanoic acid second
Ester, mixing 60 seconds.Discharging.The material mixed is crossed two-roll mill, arrives ironed for elastomeric compound roller machine
About 10mm is thick.It is cut to wide 15mm, the adhesive tape of long 220mm with bale splitter.
Embodiment 4
In 55 liters of adding pressure type banburies, add 20.0kg EP rubbers, 14.0kg butadiene rubber and 2.0kg
Polyurethane rubber.Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add
Enter 6.5kg precipitated calcium carbonate, 0.5kg alumina powder, 0.2kg zinc oxide, detergent: Butyl acetylpropanoate
0.15kg, glycol ethyl ether 0.15kg, hexachlorethane 0.15kg, plasticizer: dibutyl phthalate
0.15kg, mould release: silicone oil 0.15kg；And organic dehydration compound penetration agent: diethanolamine 0.5kg,
Catalyst carrier material: kieselguhr 0.2kg and the catalyst adsorbed: sodium tert-butoxide 0.05kg, and acetaldehyde
0.15kg.Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 0.25kg tert-butyl cumyl peroxide
Base peroxide, 0.20kg di-tert-butyl peroxide, mixing 60 seconds.Discharging.The material mistake mixed
Two-roll mill, by ironed for elastomeric compound roller machine thick to about 10mm.It is cut to wide 15mm, length with bale splitter
The adhesive tape of 220mm.
Embodiment 5
In 55 liters of adding pressure type banburies, add 21.0kg ethylene propylene diene rubber and 4.0kg acrylate rubber.
Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg dioxy
SiClx, 1.6kg Griffith's zinc white., detergent: N-methyl is than pyrrolidone 0.2kg, diethanolamine 0.2kg, plasticizer:
Di-n-butyl succinate 0.05kg, thickening material: chlorosulfonated polyethylene 2.3kg, mould release: bar wax 0.005kg
And organic dehydration compound penetration agent a group: normal propyl alcohol 1.0kg, 4A molecular sieve 1.5kg and being adsorbed
Catalyst: sulphuric acid 0.01kg；Organic dehydration compound penetration agent b group: 1,5-pentanedicarboxylic acid. 0.5kg, catalysis
Agent carrier material: natural zeolite 1.5kg and catalyst barium hydroxide 4.6kg, banburying of pressurizeing, mixing 10 minutes；
Uncap, not discharging, add 0.9kg 2,5 di-t-butyl-2,5-(di-t-butyl peroxide) hexane, mixing 60 seconds.
Discharging.The material mixed is crossed two-roll mill, by ironed for elastomeric compound roller machine thick to about 10mm.With
Bale splitter is cut to wide 15mm, the adhesive tape of long 220mm.
Embodiment 6
In 55 liters of adding pressure type banburies, add 23.0kg ethylene propylene diene rubber and 4.0kg butadiene rubber.Entirely
Journey opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg lightweight carbon
Acid calcium, 4.0kg potter's clay, 2.0kg Griffith's zinc white., detergent: N-methyl than pyrrolidone 0.2kg, diethanolamine 0.2kg,
Plasticizer: di-n-butyl succinate 0.2kg, thickening material: chlorosulfonated polyethylene 0.05kg, mould release: diformazan
Base silicone oil 0.02kg.And organic dehydration compound penetration agent a group: ethylene glycol 0.60kg, 4A molecule
Sieve 0.95kg and the phosphoric acid 0.01kg adsorbed；Organic dehydration compound penetration agent b group 1,5-pentanedicarboxylic acid. 0.3kg,
Catalyst carrier material: natural zeolite 1.0kg and catalyst: barium hydroxide 0.01kg；Organic dehydration
Compound penetrating agent c group: ethanolamine 0.73kg, catalyst carrier material: natural zeolite 0.80kg and being adsorbed
Catalyst: potassium hydroxide 0.01kg, formaldehyde 0.25kg.Pressurization banburying, mixing 10 minutes；Uncap, do not go out
Material, adds 0.9kg 2,5 di-t-butyl-2,5-(di-t-butyl peroxide) hexane, mixing 60 seconds.Discharging.?
Two-roll mill crossed by the material mixed, by ironed for elastomeric compound roller machine thick to about 10mm.Cut with bale splitter
For wide 15mm, the adhesive tape of long 220mm.
Embodiment 7
In 55 liters of adding pressure type banburies, add 10.0kg ethylene propylene diene rubber and 12.0kg butadiene rubber, 0.7kg
Acrylate rubber.Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；
Add 7.5kg precipitated calcium carbonate, 4.0kg potter's clay, 2.0kg Griffith's zinc white., detergent: N-methyl compares pyrrolidone
0.2kg, plasticizer: di-n-butyl succinate 0.2kg, thickening material: chlorosulfonated polyethylene 0.1kg, mould release:
Short chain polyethylene 0.1kg and organic dehydration compound penetration agent a group: DAA 0.30kg, 4A
Molecular sieve 0.45kg and the catalyst sodium tert-butoxide 0.04kg adsorbed；Penetrating agent b group: adipic acid 0.3kg,
Permutite 0.3kg and the catalyst barium hydroxide 0.01kg adsorbed；Penetrating agent c group ethanolamine 0.40kg,
Natural zeolite 0.40kg and the formaldehyde 0.10kg adsorbed, catalyst: sodium silicate 4.5kg；Penetrating agent d group
Ethylene glycol 0.50kg, kieselguhr 0.25kg and the catalyst sulfuric acid 0.02kg adsorbed；Add penetrating agent e group
4-hydroxy-4-methyl-2-pentanone 0.60kg, 4A molecular sieve 0.80kg and the catalyst phosphoric acid 0.07kg adsorbed.
Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 2,5 di-t-butyl-2,5-(di-t-butyl mistake
Oxygen) hexane 0.9kg, mixing 60 seconds.Discharging.The material mixed is crossed two-roll mill, elastomeric compound is used
Roller machine is ironed thick to about 10mm.It is cut to wide 15mm, the adhesive tape of long 220mm with bale splitter.
Comparative example 1: be not added with organic dehydration compound and catalyst thereof, is not added with viscosifying material, does not adds water
In 55 liters of adding pressure type banburies, add 23.0kg ethylene propylene diene rubber and 4.0kg acrylate rubber.
Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg lightweight
Calcium carbonate, 4.0kg potter's clay, 2.0kg Griffith's zinc white., N-methyl than pyrrolidone 0.2kg, diethanolamine 0.2kg,
Di-n-butyl succinate 0.2kg, short chain polyethylene 0.2kg and addition 2.5kg4A molecular sieve, 2.0kg days
So zeolite.Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 0.9kg 2,5 di-t-butyl-2,5-(two
T-butyl peroxy) hexane, mixing 60 seconds.Discharging.The material mixed is crossed two-roll mill, by elastomeric compound
Ironed thick to about 10mm with roller machine.It is cut to wide 15mm, the adhesive tape of long 220mm with bale splitter.
Comparative example 2: be not added with organic dehydration compound and catalyst thereof, is not added with viscosifying material, adds 0.43%
Water
In 55 liters of adding pressure type banburies, add 23.0kg ethylene propylene diene rubber and 4.0kg acrylate rubber.
Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg lightweight
Calcium carbonate, 4.0kg potter's clay, 2.0kg Griffith's zinc white., N-methyl than pyrrolidone 0.2kg, diethanolamine 0.2kg,
Di-n-butyl succinate 0.2kg, short chain polyethylene 0.2kg and addition 0.20kg deionized water, 2.3kg4A
Molecular sieve, 2.0kg natural zeolite.Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 0.9kg
2,5 di-t-butyl-2,5-(di-t-butyl peroxide) hexane, mixing 60 seconds.Discharging.The most double for the material mixed
Roller mill, by ironed for elastomeric compound roller machine thick to about 10mm.It is cut to wide 15mm, long 220mm with bale splitter
Adhesive tape.
Comparative example 3: be not added with organic dehydration compound and catalyst thereof, is not added with viscosifying material, adds 4.28%
Water
In 55 liters of adding pressure type banburies, add 23.0kg ethylene propylene diene rubber and 4.0kg acrylate rubber.
Whole process opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 7.5kg lightweight
Calcium carbonate, 4.0kg potter's clay, 2.0kg Griffith's zinc white., N-methyl than pyrrolidone 0.2kg, diethanolamine 0.2kg,
Di-n-butyl succinate 0.2kg, short chain polyethylene 0.2kg and addition 2.0kg deionized water, 1.5kg4A
Molecular sieve, 1.0kg natural zeolite.Pressurization banburying, mixing 10 minutes；Uncap, not discharging, add 0.9kg
2,5 di-t-butyl-2,5-(di-t-butyl peroxide) hexane, mixing 60 seconds.Discharging.The most double for the material mixed
Roller mill, by ironed for elastomeric compound roller machine thick to about 10mm.It is cut to wide 15mm, long 220mm with bale splitter
Adhesive tape.
Comparative example 4: the product before improvement
In 55 liters of adding pressure type banburies, add 20.0kg butadiene rubber and 7.0kg ethylene propylene diene rubber.Entirely
Journey opens chuck cooling water cooling, makes temperature be less than 90 DEG C, mixing 3 minutes；Add 0.54kg titanium dioxide
Titanium, 10.0kg silicon dioxide, 1.0kg precipitated calcium carbonate, 1.0kg potter's clay, bar wax 0.03kg, silicone oil 0.02kg.
N-methyl is than pyrrolidone 0.2kg, di-n-butyl succinate 0.2kg, ethylene glycol butyl ether 0.2kg, imidazoles
2.0kg, diethylenetriamine 0.1kg, triethanolamine 0.1kg, diethanolamine 0.1kg, dimethyl sulfoxide 0.1kg,
Glycol ethyl ether 0.1kg, monoethanolamine 0.1kg, DAA 0.1kg, isopropylideneacetone 0.1kg,
Ethyl levulinate 0.5kg, Butyl acetylpropanoate 0.5kg, hexachlorethane 0.1kg, 1,1,1 trichloroethane
0.1kg, cumene 0.1kg, diisopropyl benzene 0.1kg, 4-amido amylalcohol 0.1kg, oxazolidine 0.1kg,
Dimethyl oxazolidine 0.1kg, dioxane 0.1kg, oxolane 0.1kg, pressurization banburying, mixing 10 points
Clock；Uncap, not discharging, add 1.3kg cumyl peroxide, mixing 60 seconds.Discharging.Mixing
Two-roll mill crossed by good material, by ironed for elastomeric compound roller machine thick to about 10mm.It is cut to width with bale splitter
15mm, the adhesive tape of long 220mm.
Interpretation of result: the performance test data such as table of the adhesive tape that embodiment 1～7 and comparative example 1～4 prepare
Shown in 1.
Table 1
From the data of table 1 it will be seen that the adhesive tape ripening intensity for preparing of the present invention is good, without fractureing and falling bits,
Can cleaning mold, the excellent effect of 4 clear moulds completely, clear mould number of times can be reduced, improve and imitate clearly rate.
Claims (8)
1. a unvulcanized rubber composition, it is characterised in that include rubber, peroxide vulcanizing system, fill out
Charge, plasticizer, mould release, detergent, enhancing clean organic compound penetrating agent and the catalysis thereof of effect
Agent and carrier material thereof；
Described rubber is selected from the combination of unsaturated non-polar rubber with saturated nonpolar rubber；Its usage amount is described
The 50～80wt% of unvulcanized rubber composition total amount；
Described enhancing is cleaned the organic compound penetrating agent of effect and is included at least one of following raw material:
130～180 DEG C of compounds that dehydration can occur, including following several: (1) alcohol catalysis anhydro compounds:
Normal propyl alcohol, 4-hydroxy-4-methyl-2-pentanone, ethylene glycol；(2) carboxylic acid catalytic dehydration compound: adipic acid,
1,5-pentanedicarboxylic acid.；(3) alcohol amine compound and aldehydes anhydro compounds: ethanolamine, diethanolamine, 2-amino-2-second
Base-1,3-propylene glycol, 2-amino-2-methyl-1-propanol, formaldehyde, propionic aldehyde；Its usage amount is described unvulcanized rubber
The 0.1～10wt% of glue composition total amount；
Described catalyst is: sulphuric acid, nitric acid, hydrochloric acid, phosphoric acid, ethylsulfonic acid, pyrovinic acid, to toluene sulphur
Acid, boric acid, potassium hydroxide, sodium hydroxide, barium hydroxide, sodium silicate, potassium tert-butoxide, sodium tert-butoxide,
At least one of iodine；Its usage amount is the 0.01～10wt% of described unvulcanized rubber composition total amount；
Described carrier material is: molecular sieve, kieselguhr, natural zeolite, permutite at least one；It makes
Consumption is the 1～10wt% of described unvulcanized rubber composition total amount.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described rubber is: fourth
Benzene rubber, butadiene rubber, EP rubbers, polyurethane rubber, at least two kinds of acrylate rubber.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described peroxide sulfur
Change system is: cumyl peroxide, di-tert-butyl peroxide, peroxidized t-butyl perbenzoate, peroxide
At least one of change tert-butyl cumyl peroxide；Its usage amount is described unvulcanized rubber composition total amount
2～5wt%.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described inserts is:
Pulvis Talci, activated clay, silicon dioxide powder, alumina powder, oxide powder and zinc, precipitated calcium carbonate, potter's clay,
Calcium silicates, calcium aluminate, magnesium carbonate, barium sulfate, titanium dioxide, Griffith's zinc white. at least one；Its usage amount
For described unvulcanized rubber composition total amount 16～40wt%.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described plasticizer is:
Stearic acid, dodecylic acid, di-n-butyl succinate, dibutyl phthalate, liquid paraffin at least one；
Its usage amount is the 0.1～5wt% of described unvulcanized rubber composition total amount.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described mould release is:
Bar wax, short chain polyethylene, paraffin, silicone oil at least one；Its usage amount is described unvulcanized rubber composition
The 0.01～5wt% of thing total amount.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described detergent be with
At least one in lower raw material: N-Methyl pyrrolidone, dimethyl sulfoxide, glycol ethyl ether, ethylene glycol
Monobutyl ether, triethanolamine, diethylenetriamine, DAA, Mesityl oxide, ethyl levulinate,
Butyl acetylpropanoate, hexachlorethane, 1,1,1-trichloroethane, cumene, diisopropyl benzene, 4-amino penta
Alcohol, Ketocyclopentane, Ketohexamethylene；Five yuan, 6-membered heterocyclic compound and derivant thereof: imidazoles, Methylimidazole.,
Oxazole, oxazolidine, dimethyl oxazolidine, dioxane, furan, oxolane；Its usage amount is described
The 0.1～5wt% of unvulcanized rubber composition total amount.
Unvulcanized rubber composition the most according to claim 1, it is characterised in that described compositions is also wrapped
Including thickening material, described thickening material is: in chlorosulfonated polyethylene, boric acid, coumarone, Colophonium at least
A kind of；Its usage amount is the 0.1～5wt% of unvulcanized rubber composition total amount.
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| CN104804241A (en) * | 2015-04-29 | 2015-07-29 | 海太半导体（无锡）有限公司 | Semiconductor high-viscosity film injection cleaning material |
| CN107011553A (en) * | 2017-05-04 | 2017-08-04 | 天津德高化成新材料股份有限公司 | A kind of rubber mould exempts from dismounting mold cleaning material and preparation method thereof with online |
| CN109957186A (en) * | 2017-12-22 | 2019-07-02 | 四川素恩吉科技有限公司 | A kind of mold composition |
| CN108047694A (en) * | 2017-12-27 | 2018-05-18 | 东莞市浦元电子有限公司 | Semiconductor packaging mold cleaning material and preparation method thereof |
| CN109849244B (en) * | 2019-03-11 | 2019-12-13 | 广东四会互感器厂有限公司 | Method for descaling pressure gel mold |
| CN114058127A (en) * | 2021-11-30 | 2022-02-18 | 苏州赛伍应用技术股份有限公司 | Clean and moist membrane adhesive tape and preparation method and application thereof |
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| CN1403562A (en) * | 2002-10-18 | 2003-03-19 | 成都飞机工业（集团）有限责任公司 | Rubber mold cleaning size material |
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| CN102766284A (en) * | 2012-08-07 | 2012-11-07 | 天津德高化成电子材料有限公司 | Tasteless mold cleaning material for semiconductor packaging mold |
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| CN1403562A (en) * | 2002-10-18 | 2003-03-19 | 成都飞机工业（集团）有限责任公司 | Rubber mold cleaning size material |
| CN1727387A (en) * | 2004-07-28 | 2006-02-01 | 纳拉化学株式会社 | Rubber compsns. for cleaning and stripping mould |
| CN102775656A (en) * | 2012-07-15 | 2012-11-14 | 湖州师范学院 | Rubber composition used for cleaning integrated circuit (IC) die |
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