CN108976807A - A kind of preparation method of high-temp resisting high-humidity resisting mold glue - Google Patents
A kind of preparation method of high-temp resisting high-humidity resisting mold glue Download PDFInfo
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- CN108976807A CN108976807A CN201810668172.4A CN201810668172A CN108976807A CN 108976807 A CN108976807 A CN 108976807A CN 201810668172 A CN201810668172 A CN 201810668172A CN 108976807 A CN108976807 A CN 108976807A
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- 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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Abstract
The present invention relates to a kind of preparation methods of high-temp resisting high-humidity resisting mold glue, belong to technical field of rubber material.The present invention utilizes organic-silicon-modified methyl vinyl silicone rubber, and the heat resistance and surface property of methyl vinyl silicone rubber can be improved；Organo montmorillonite is a kind of typical 2: 1 type phyllosilicate, it is compound nanoscale to be carried out with methyl vinyl silicone rubber, there is very strong active force between the two, hydroxyl and methyl vinyl silicone rubber polarity of chain Interaction of substituents on organo montmorillonite lamella, increase the interaction between montmorillonite and methyl vinyl silicone rubber, strand is set preferably to be inserted between organo montmorillonite lamella, strut piece interlamellar spacing, and then it is dispersed in organo montmorillonite in methyl vinyl silicone rubber matrix, to which the heat resistance of composite material can be improved, tensile strength and elongation at break etc.；Methyl vinyl silicone rubber, organosilicon are combined with organo montmorillonite, preparation has both the material of three's excellent performance.
Description
Technical field
The present invention relates to a kind of preparation methods of high-temp resisting high-humidity resisting mold glue, belong to technical field of rubber material.
Background technique
Silica gel, also referred to as silicon rubber have many advantages, such as that high temperature resistant, corrosion-resistant, tear resistance is strong, simulation accuracy is high, therefore quilt
It is widely used in the manufacture of materials such as craftwork and cultural stone mould.
It is known as mold glue dedicated for the silica gel of production of crafts mould, generally uses room temperature vulcanized silicone rubber (abbreviation RTV)
Manufacture.RTV is a kind of macromolecular elastomer, it is using silicon atom and oxygen atom as the synthetic material of skeleton, on each silicon atom
It is a kind of fibrous polymer polymer with Si-O-Si chain belt containing 1~2 organic group (mainly methyl).Cause
This, RTV has the property that good chemical stability, nontoxic, non-corrosive；Good fluidity can be full of mold automatically；It can
Curingprocess rate is controlled, is vulcanized under room temperature normal pressure, convenient for operating good release property；Simulation quality is strong, and decorative pattern is true to nature；Molding speed
Fastly, it can be made into mold in general 20 hours.
Mold glue is divided into Addition-type mold rubber and condensed type mold glue, and condensed type mold glue has superior mobility and takes off
Mould, easy to operate, die size is stablized, and the features such as heat-resisting, chemicals-resistant, good physical performance and high tear strength, especially uses
In unsaturated polyester product, durability is good, and die life is long, but condensed type mold glue can generate in process of production it is low
Molecular substance, such as methanol can bring pollution, not environmentally；Add-on type mold has transparency good, is easy deep cure, shrinks
The small feature of rate is mainly used for the production of precision die and exquisite duplicate.
Silicone molding rubber since multiple mould precision is high, and have good simulation quality, release property, excellent flexibility,
The advantages such as molding is simple and cheap and emerge rapidly, largely substitute gypsum, metal and timber, become the important of Mold Making
One of material.It is widely used in the fields such as Art Stone, photoelectricity equipment, household electrical appliance, auto parts, toy.But production application
In the process, especially under the condition of high temperature and high humidity, that there are shrinking percentages is larger for mold glue, and turning deviation is big and intensity is poor, ruler
The deficiencies of very little stability is lower, causes die life shorter, substantially increases the production cost of enterprise.
Summary of the invention
The technical problems to be solved by the invention: for mold glue under the condition of high temperature and high humidity, that there are shrinking percentages is larger, turns
The problem that angular displacement is big and intensity is poor provides a kind of preparation method of high-temp resisting high-humidity resisting mold glue.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) 1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed with dehydrated alcohol by volume, 10~12h of magnetic agitation, it is heavy to stand
Change 12h, is centrifugated and dry, is ground after being cooled to room temperature, obtain nanometer powder；According to parts by weight, 1~5 part is weighed respectively
Nanometer powder, 0.2~0.7 part of dehydrated alcohol, 0.7~0.9 part of positive silane ethyl ester, 0.4~0.6 part of mass fraction are 37% hydrochloric acid,
It is 37% hydrochloric acid, stirring 18 that dehydrated alcohol, silylating reagent, ethyl orthosilicate and mass fraction are added in SiO 2 powder
~20h obtains modified Nano material；
(2) according to parts by weight, 2~4 parts of sodium-based montmorillonites, 40~50 parts of deionized waters, 3~5 parts of double octadecanes are weighed respectively
Sodium-based montmorillonite and deionized water decentralized processing are obtained dispersion liquid A by base alkyl dimethyl ammonium chloride, 20~30 parts of dehydrated alcohols；It will be double
Octadecyldimethyl chloride leach obtains solution B in dehydrated alcohol；Dispersion liquid A and solution B are mixed, in 70~80 DEG C
It is filtered after 10~12h of lower high-speed stirred, obtains filter cake, filter cake is washed with deionized water to filtrate detection without filtering after must washing after precipitating
Filter cake after washing is dried under vacuum to constant weight, grind into powder in 100 DEG C by cake, and sieving obtains organo montmorillonite；
(3) according to parts by weight, 20~40 parts of organo montmorillonites, 30~40 parts of methyl vinyl silicone rubbers, 1~3 are weighed respectively
Part catalyst chloroplatinic acid, 10~20 parts of vinyl-terminated silicone fluids, 2~10 parts of white carbon blacks, 1~4 part of modified Nano material, 2~3 parts it is solid
Organo montmorillonite and methyl vinyl silicone rubber are placed in 15~30min of grinding in three-roller, catalyst are added by agent triethylamine
Chloroplatinic acid, modified Nano material and white carbon black, at 85 DEG C stir 3~4h after, be added vinyl-terminated silicone fluid, continue stirring 4~
5h, is added curing agent and is poured after mixing in a mold, and solidification obtains the mold glue.
Centrifuge separation described in step (1) and drying steps are as follows: 5~10min is centrifugated at 2000~2500r/min
Afterwards, 50~60 DEG C of 10~12h of oven drying are placed in.
Decentralized processing described in step (2) is that 0.5~1h is stirred at 3000~4000r/min.
The AgNO of 0.1mol/L is used in the detection of filtrate described in step (2) without precipitating3Solution detection.
It is 300~400 mesh that grit number is crossed described in step (2).
Condition of cure described in step (3) is to be poured vacuum defoamation in a mold after mixing, at 90~100 DEG C
In baking oven solidification 20~for 24 hours.
The present invention is compared with other methods, and advantageous effects are:
The present invention has the characteristics that low-surface-energy, high-low temperature resistant, weatherability, hydrophobicity using organosilicon, with organic-silicon-modified first
The heat resistance and surface property of methyl vinyl silicone rubber can be improved in base vinylsiloxane rubber；Organo montmorillonite is a kind of typical case
2: 1 type phyllosilicates, can with methyl vinyl silicone rubber carry out nanoscale it is compound, between the two have very strong effect
Power, hydroxyl and methyl vinyl silicone rubber polarity of chain Interaction of substituents on organo montmorillonite lamella, increases illiteracy
Interaction between de- soil and methyl vinyl silicone rubber, enable strand be preferably inserted into organo montmorillonite lamella it
Between, piece interlamellar spacing is strutted, and then be dispersed in organo montmorillonite in methyl vinyl silicone rubber matrix, so that composite wood can be improved
Heat resistance, tensile strength and elongation at break of material etc.；Methyl vinyl silicone rubber, organosilicon are risen in conjunction with organo montmorillonite
Come, preparation has both the material of three's excellent performance.
Specific embodiment
1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed with dehydrated alcohol by volume, 10~12h of magnetic agitation, it is heavy to stand
Change 12h, after being centrifugated 5~10min at 2000~2500r/min, is placed in 50~60 DEG C of 10~12h of oven drying, it is cooling
It is ground after to room temperature, obtains SiO 2 powder；According to parts by weight, 1~5 part of SiO 2 powder, 0.2~0.7 are weighed respectively
Part dehydrated alcohol, 0.7~0.9 part of positive silane ethyl ester, 0.4~0.6 part of mass fraction are 37% hydrochloric acid, in SiO 2 powder
It is 37% hydrochloric acid that dehydrated alcohol, silylating reagent, ethyl orthosilicate and mass fraction, which is added, stirs 18~20h, obtains modified Nano
Material；According to parts by weight, 2~4 parts of sodium-based montmorillonites, 40~50 parts of deionized waters, 3~5 parts of double octadecyls are weighed respectively
Alkyl dimethyl ammonium chloride, 20~30 parts of dehydrated alcohols, disperse sodium-based montmorillonite in deionized water, in 3000~4000r/min
0.5~1h of lower stirring, obtains dispersion liquid A；Dioctadecyl dimethyl ammonium chloride is dissolved in dehydrated alcohol, solution B is obtained；It will divide
Dispersion liquid A and solution B mixing, filter after 10~12h of high-speed stirred at 70~80 DEG C, obtain filter cake, filter cake be washed with deionized water to
Filtrate is with the AgNO of 0.1mol/L3Solution detection is dried in vacuo without filter cake after precipitating to wash, by the filter cake after washing in 100 DEG C
To constant weight, grind into powder, sieving obtains organo montmorillonite；According to parts by weight, weigh respectively 20~40 parts of organo montmorillonites,
30~40 parts of methyl vinyl silicone rubbers, 1~3 part of catalyst chloroplatinic acid, 10~20 parts of vinyl-terminated silicone fluids, 2~10 parts of hard charcoals
Black, 1~4 part of modified Nano material, 2~3 parts of curing agent triethylamines, are placed in three for organo montmorillonite and methyl vinyl silicone rubber
15~30min is ground in roller machine, catalyst chloroplatinic acid, modified Nano material and white carbon black is added, and 3~4h is stirred at 85 DEG C
Afterwards, vinyl-terminated silicone fluid is added, continues 4~5h of stirring, curing agent is added and is poured vacuum defoamation in a mold after mixing,
In 90~100 DEG C of baking oven solidification 20~for 24 hours, obtain mold glue described in high-temp resisting high-humidity resisting.
1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed by volume, magnetic agitation 10h with dehydrated alcohol, stands precipitation
12h is placed in 50 DEG C of oven drying 10h, grinds after being cooled to room temperature, obtain titanium dioxide after being centrifugated 5min at 2000r/min
Si powder；According to parts by weight, 1 part of SiO 2 powder, 0.2 part of dehydrated alcohol, 0.7 part of positive silane ethyl ester, 0.4 are weighed respectively
Part mass fraction is 37% hydrochloric acid, and dehydrated alcohol, silylating reagent, ethyl orthosilicate and quality are added in SiO 2 powder
Score is 37% hydrochloric acid, stirs 18h, obtains modified Nano material；According to parts by weight, 2 parts of sodium-based montmorillonites, 40 parts are weighed respectively
Deionized water, 3 parts of dioctadecyl dimethyl ammonium chlorides, 20 parts of dehydrated alcohols, disperse sodium-based montmorillonite in deionized water,
0.5h is stirred at 3000r/min, obtains dispersion liquid A；Dioctadecyl dimethyl ammonium chloride is dissolved in dehydrated alcohol, is obtained molten
Liquid B；Dispersion liquid A and solution B are mixed, filtered after high-speed stirred 10h at 70 DEG C, obtains filter cake, filter cake be washed with deionized water to
Filtrate is with the AgNO of 0.1mol/L3Solution detection is dried in vacuo without filter cake after precipitating to wash, by the filter cake after washing in 100 DEG C
To constant weight, grind into powder, sieving obtains organo montmorillonite；According to parts by weight, 20 parts of organo montmorillonites, 30 parts are weighed respectively
Methyl vinyl silicone rubber, 1 part of catalyst chloroplatinic acid, 10 parts of vinyl-terminated silicone fluids, 2 parts of white carbon blacks, 1 part of modified Nano material, 2
Part curing agent triethylamine, organo montmorillonite and methyl vinyl silicone rubber are placed in three-roller and grind 15min, and catalyst is added
After stirring 3h at 85 DEG C, vinyl-terminated silicone fluid is added in chloroplatinic acid, modified Nano material and white carbon black, is continued to stir 4h, is added
Curing agent is poured in a mold after mixing, and vacuum defoamation solidifies 20h in 90 DEG C of baking oven, obtains the high-temp resisting high-humidity resisting
Mold glue.
1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed by volume, magnetic agitation 11h with dehydrated alcohol, stands precipitation
12h is placed in 55 DEG C of oven drying 11h, grinds after being cooled to room temperature, obtain titanium dioxide after being centrifugated 7min at 2250r/min
Si powder；According to parts by weight, 3 parts of SiO 2 powders, 0.5 part of dehydrated alcohol, 0.8 part of positive silane ethyl ester, 0.5 are weighed respectively
Part mass fraction is 37% hydrochloric acid, and dehydrated alcohol, silylating reagent, ethyl orthosilicate and quality are added in SiO 2 powder
Score is 37% hydrochloric acid, stirs 19h, obtains modified Nano material；According to parts by weight, 3 parts of sodium-based montmorillonites, 45 parts are weighed respectively
Deionized water, 4 parts of dioctadecyl dimethyl ammonium chlorides, 25 parts of dehydrated alcohols, disperse sodium-based montmorillonite in deionized water,
0.75h is stirred at 3500r/min, obtains dispersion liquid A；Dioctadecyl dimethyl ammonium chloride is dissolved in dehydrated alcohol, is obtained
Solution B；Dispersion liquid A and solution B are mixed, is filtered after high-speed stirred 11h at 75 DEG C, obtains filter cake, filter cake is washed with deionized water
To filtrate with the AgNO of 0.1mol/L3Solution detection does the filter cake after washing in 100 DEG C of vacuum without filter cake after precipitating to wash
It is dry to constant weight, grind into powder, sieving obtains organo montmorillonite；According to parts by weight, 30 parts of organo montmorillonites, 35 are weighed respectively
Part methyl vinyl silicone rubber, 2 parts of catalyst chloroplatinic acids, 15 parts of vinyl-terminated silicone fluids, 6 parts of white carbon blacks, 3 parts of modified Nano materials
Material, 2 parts of curing agent triethylamines, organo montmorillonite and methyl vinyl silicone rubber are placed in three-roller and grind 22min, addition is urged
After stirring 4h at 85 DEG C, vinyl-terminated silicone fluid is added in agent chloroplatinic acid, modified Nano material and white carbon black, continues to stir 4h,
Curing agent is added to be poured after mixing in a mold, vacuum defoamation solidifies 22h in 95 DEG C of baking oven, obtains the high temperature resistant
High humidity mold glue.
1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed by volume, magnetic agitation 12h with dehydrated alcohol, stands precipitation
12h is placed in 60 DEG C of oven drying 12h, grinds after being cooled to room temperature, obtain dioxy after being centrifugated 10min at 2500r/min
SiClx powder；According to parts by weight, weigh respectively 5 parts of SiO 2 powders, 0.7 part of dehydrated alcohol, 0.9 part of positive silane ethyl ester,
0.6 part of mass fraction is 37% hydrochloric acid, and dehydrated alcohol, silylating reagent, ethyl orthosilicate and matter are added in SiO 2 powder
Amount score is 37% hydrochloric acid, stirs 20h, obtains modified Nano material；According to parts by weight, 4 parts of sodium-based montmorillonites, 50 are weighed respectively
Part deionized water, 5 parts of dioctadecyl dimethyl ammonium chlorides, 30 parts of dehydrated alcohols, disperse deionized water for sodium-based montmorillonite
In, 1h is stirred at 4000r/min, obtains dispersion liquid A；Dioctadecyl dimethyl ammonium chloride is dissolved in dehydrated alcohol, is obtained
Solution B；Dispersion liquid A and solution B are mixed, is filtered after high-speed stirred 12h at 80 DEG C, obtains filter cake, filter cake is washed with deionized water
To filtrate with the AgNO of 0.1mol/L3Solution detection does the filter cake after washing in 100 DEG C of vacuum without filter cake after precipitating to wash
It is dry to constant weight, grind into powder, sieving obtains organo montmorillonite；According to parts by weight, 40 parts of organo montmorillonites, 40 are weighed respectively
Part methyl vinyl silicone rubber, 3 parts of catalyst chloroplatinic acids, 20 parts of vinyl-terminated silicone fluids, 10 parts of white carbon blacks, 4 parts of modified Nano materials
Material, 3 parts of curing agent triethylamines, organo montmorillonite and methyl vinyl silicone rubber are placed in three-roller and grind 30min, addition is urged
After stirring 4h at 85 DEG C, vinyl-terminated silicone fluid is added in agent chloroplatinic acid, modified Nano material and white carbon black, continues to stir 5h,
Curing agent is added to be poured after mixing in a mold, vacuum defoamation solidifies for 24 hours in 100 DEG C of baking oven, obtains the high temperature resistant
High humidity mold glue.
The mold glue that high-temp resisting high-humidity resisting mold glue prepared by the present invention and Shandong company produce is detected, it is specific to examine
It is as follows to survey result:
(1) Mechanics Performance Testing:
It is high-temp resisting high-humidity resisting mold glue tensile strength prepared by the present invention, disconnected in the environment of 200 DEG C of temperature, relative humidity are 60%
Split elongation, 300% stress at definite elongation is measured by GB/T528-2009；Tearing strength is measured by GB/T529-2008；Wherein stretch
The each formula of intensity, elongation at break, tearing strength, 300% stress at definite elongation cuts 5 test pieces, is averaged after test.
1 high-temp resisting high-humidity resisting mold glue performance characterization of table
As shown in Table 1, high-temp resisting high-humidity resisting mold glue prepared by the present invention, elongation at break is high, and angle tear strength is big, lancinating
It can be improved, further increase the mechanical performance of mold glue, there is preferable prospect of the application.
Claims (6)
1. a kind of preparation method of high-temp resisting high-humidity resisting mold glue, which is characterized in that specific steps are as follows:
(1) 1: 0.5: 5 ethyl orthosilicate, ammonium hydroxide are mixed with dehydrated alcohol by volume, 10~12h of magnetic agitation, it is heavy to stand
Change 12h, is centrifugated and dry, is ground after being cooled to room temperature, obtain nanometer powder；According to parts by weight, 1~5 part is weighed respectively
Nanometer powder, 0.2~0.7 part of dehydrated alcohol, 0.7~0.9 part of positive silane ethyl ester, 0.4~0.6 part of mass fraction are 37% hydrochloric acid,
It is 37% hydrochloric acid, stirring 18 that dehydrated alcohol, silylating reagent, ethyl orthosilicate and mass fraction are added in SiO 2 powder
~20h obtains modified Nano material；
(2) according to parts by weight, 2~4 parts of sodium-based montmorillonites, 40~50 parts of deionized waters, 3~5 parts of double octadecanes are weighed respectively
Sodium-based montmorillonite and deionized water decentralized processing are obtained dispersion liquid A by base alkyl dimethyl ammonium chloride, 20~30 parts of dehydrated alcohols；It will be double
Octadecyldimethyl chloride leach obtains solution B in dehydrated alcohol；Dispersion liquid A and solution B are mixed, in 70~80 DEG C
It is filtered after 10~12h of lower high-speed stirred, obtains filter cake, filter cake is washed with deionized water to filtrate detection without filtering after must washing after precipitating
Filter cake after washing is dried under vacuum to constant weight, grind into powder in 100 DEG C by cake, and sieving obtains organo montmorillonite；
(3) according to parts by weight, 20~40 parts of organo montmorillonites, 30~40 parts of methyl vinyl silicone rubbers, 1~3 are weighed respectively
Part catalyst chloroplatinic acid, 10~20 parts of vinyl-terminated silicone fluids, 2~10 parts of white carbon blacks, 1~4 part of modified Nano material, 2~3 parts it is solid
Organo montmorillonite and methyl vinyl silicone rubber are placed in 15~30min of grinding in three-roller, catalyst are added by agent triethylamine
Chloroplatinic acid, modified Nano material and white carbon black, at 85 DEG C stir 3~4h after, be added vinyl-terminated silicone fluid, continue stirring 4~
5h, is added curing agent and is poured after mixing in a mold, and solidification obtains the mold glue.
2. a kind of preparation method of high-temp resisting high-humidity resisting mold glue according to claim 1, it is characterised in that: step (1) institute
The centrifuge separation stated and drying steps are as follows: after being centrifugated 5~10min at 2000~2500r/min, be placed in 50~60 DEG C of bakings
Case dries 10~12h.
3. a kind of preparation method of high-temp resisting high-humidity resisting mold glue according to claim 1, it is characterised in that: step (2) institute
The decentralized processing stated is that 0.5~1h is stirred at 3000~4000r/min.
4. a kind of preparation method of high-temp resisting high-humidity resisting mold glue according to claim 1, it is characterised in that: step (2) institute
The AgNO of 0.1mol/L is used in the filtrate detection stated without precipitating3Solution detection.
5. a kind of preparation method of high-temp resisting high-humidity resisting mold glue according to claim 1, it is characterised in that: step (2) institute
The grit number of crossing stated is 300~400 mesh.
6. a kind of preparation method of high-temp resisting high-humidity resisting mold glue according to claim 1, it is characterised in that: step (3) institute
The condition of cure stated is to be poured vacuum defoamation in a mold after mixing, in 90~100 DEG C of baking oven solidify 20~for 24 hours.
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| CN201810668172.4A CN108976807A (en) | 2018-06-26 | 2018-06-26 | A kind of preparation method of high-temp resisting high-humidity resisting mold glue |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831084A (en) * | 2010-06-03 | 2010-09-15 | 天津大学 | Organically-modified MMT and cross-linking method for high-temperature silicon disulfide rubber |
| CN102181158A (en) * | 2011-03-04 | 2011-09-14 | 上海工程技术大学 | Montmorillonite-modified silicon rubber nanocomposite and preparation method thereof |
| CN103275495A (en) * | 2013-05-27 | 2013-09-04 | 上海工程技术大学 | Composite flame-retardant silicone rubber material with high thermal stability and preparation method thereof |
| CN104987727A (en) * | 2015-07-20 | 2015-10-21 | 上海工程技术大学 | Preparation method for silicon rubber containing organically modified montmorillonite |
-
2018
- 2018-06-26 CN CN201810668172.4A patent/CN108976807A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831084A (en) * | 2010-06-03 | 2010-09-15 | 天津大学 | Organically-modified MMT and cross-linking method for high-temperature silicon disulfide rubber |
| CN102181158A (en) * | 2011-03-04 | 2011-09-14 | 上海工程技术大学 | Montmorillonite-modified silicon rubber nanocomposite and preparation method thereof |
| CN103275495A (en) * | 2013-05-27 | 2013-09-04 | 上海工程技术大学 | Composite flame-retardant silicone rubber material with high thermal stability and preparation method thereof |
| CN104987727A (en) * | 2015-07-20 | 2015-10-21 | 上海工程技术大学 | Preparation method for silicon rubber containing organically modified montmorillonite |
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Application publication date: 20181211 |