CN107236490A - A kind of preparation method of high temperature resistant pressure sensitive adhesive - Google Patents
A kind of preparation method of high temperature resistant pressure sensitive adhesive Download PDFInfo
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- CN107236490A CN107236490A CN201710510242.9A CN201710510242A CN107236490A CN 107236490 A CN107236490 A CN 107236490A CN 201710510242 A CN201710510242 A CN 201710510242A CN 107236490 A CN107236490 A CN 107236490A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
The invention discloses a kind of preparation method of high temperature resistant pressure sensitive adhesive, belong to technical field of adhesive preparation.The present invention first passes through hydrochloric acid decomposition method and the Silica hydrogel containing abundant silicone hydroxyl is made, silicic acid salt treatment zeolite is used again, zeolite surface is set to carry silicone hydroxyl, make catalyst with the concentrated sulfuric acid again, the silicone hydroxyl of Silica hydrogel and zeolite surface is set to occur dehydration condensation, form the great Si O Si keys of bond energy, it is more than C C keys and C O keys in general organic matter due to the bond energy of Si O Si keys, with good heat-resisting quantity, use natural resin in the presence of microorganism to filler modified again, increase the quantity of filler surface natural resin particle, improve the compatibility between high temperature resistant filler and acrylate, and the natural resin of these low melting points can be melted in advance in the case where running into high temperature, absorb partial heat, further improve the heat-resisting quantity of pressure sensitive adhesive, the obtained pressure sensitive adhesive pliability of the present invention and high-temperature stability are splendid, have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of high temperature resistant pressure sensitive adhesive, belong to technical field of adhesive preparation.
Background technology
Pressure sensitive adhesive full name is pressure-sensitive adhesive, and abbreviation pressure sensitive adhesive the characteristics of due to being difficult solid, is also commonly called as not doing
Glue.Pressure sensitive adhesive is one of current maximum adhesive kind of most widely used, yield, with daily life relation is close can not
Point.It is one kind in bonding process to pressure-sensitive adhesive, under the effect of less pressure, it is not necessary to which heating is molten
The effect of agent can just form firm bonding.It is be bonded that pressure sensitive adhesive and bonded object surface rely primarily on Van der Waals force progress, because
This has several big obvious advantages：（1）Bonding process is easy；（2）Peel and be also easy to；（3）Stripping will not destroy gluing of surfaces
Structure；（4）Glue-line is stable, and the bonding time is long.
Pressure sensitive adhesive species is more, and pressure sensitive adhesive product is segmented into polytype according to different criteria for classifications.From pressure sensitive adhesive
Main component distinguish, polyacrylate pressure-sensitive, rubber pressure-sensitive adhesive, thermoplastic elastomer pressure sensitive adhesive and poly- can be divided into
Urethane pressure sensitive adhesive etc..Because acrylate pressure-sensitive adhesive is fast light, ageing-resistant and water resistance is preferable, and with excellent pressure-sensitive
Property and cohesive, performance is stable, is widely used in many fields such as building, electrical equipment, traffic, medical treatment, packaging, health,
Therefore the main focus of pressure sensitive adhesive research field is turned into recent years.
But acrylate pressure-sensitive adhesive high-temperature stability is general all poor, and it is difficult to be bonded low energy surface material,
Degumming phenomenon is easily produced under hot environment more than 150 DEG C.For these problems, researcher is with butyl acrylate, acetic acid
Vinyl acetate, acrylic monomers are matrix, using DAAM/adipic dihydrazide external crosslinking system, by emulsification and
Semi-continuous charging technique is prepared for external crosslinking type acrylate emulsion, though this method improves product to a certain extent
Resistance to elevated temperatures, but also deposit easy degumming in high temperature environments, the problem of holding sticky poor.Therefore a kind of high temperature resistant type third is invented
Olefin(e) acid ester pressure-sensitive has positive meaning to pressure sensitive adhesive preparing technical field.
The content of the invention
Present invention mainly solves technical problem, for current acrylate pressure-sensitive adhesive, although fast light, resistance to ag(e)ing is good, but
It is that high-temperature stability is general all poor, and is difficult to be bonded low energy surface material, under the hot environment more than 150 DEG C easily
There is provided a kind of preparation method of high temperature resistant pressure sensitive adhesive for the defect of generation degumming phenomenon.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）Sodium silicate solution and sodium chloride solution are fitted into beaker, beaker refrigerator is put into after stirring mixing, at 2~4 DEG C
Saltout 3~5h, waits end of saltouing, and continues to add hydrochloric acid into beaker, 2~3h of stirring reaction, is separated by filtration removal filtrate, obtains
Gel-like product；
（2）Zeolite powder is poured into lithium metasilicate solution, sonic oscillation processing is filtrated to get filter residue, by filter residue and above-mentioned gel
It is fitted into after the mixing of shape product in three-necked flask, then is added dropwise into flask after sulfuric acid solution, completion of dropping in immigration water-bath, heating
60~70 DEG C are warming up to, 3~5h of stirring reaction, reaction is filtered after terminating, isolated filter cake discharges after freeze-drying, produced
Make high temperature resistant filler by oneself；
（3）Weigh on 50~60g beeswaxs, 20~30g peach gums, 30~40g gum arabics, 70~80g rosin and 300~400g
Self-control high temperature resistant filler mixed grinding is stated, then the material after grinding is transferred in fermentation tank, withered grass gemma is added into fermentation tank
Bacillus bacteria suspension, after stirring, sealing and fermenting；
（4）Treat after the completion of above-mentioned fermentation, be filtrated to get filter residue, first by the 15~20min that sterilized at 110~120 DEG C of filter residue, then freeze
Dry, obtain modified, high temperature resistant filler, it is standby；
（5）0.3~0.5g lauryl sodium sulfate, 1.3~1.5g NPEs and 50 are added into four-hole boiling flask
~100mL deionized waters, added after stirring 30~35g ethyl acrylates, 2.2~3.0g hydroxy-ethyl acrylates, 2.5~
3.6g Isooctyl acrylate monomers and 1.5~2.0g methacrylic acids, four-hole boiling flask is moved into 60~70 DEG C of water-baths, is protected in nitrogen
Under shield, 30~40min of insulated and stirred obtains pre-emulsion；
（6）Above-mentioned four-hole boiling flask is moved into oil bath pan, then 0.4~0.8g potassium peroxydisulfates, stirring reaction are added to four-hole boiling flask
0.6~1.2g potassium peroxydisulfates are added after 10~15min, continue 2~4h of insulation reaction, after question response terminates, reaction production are obtained
Thing, adjusts reactant pH to 7.0~8.0 with ammoniacal liquor, produces Acrylate pressure-sensitive adhesive emulsion；
（7）By emulsifier op-10, step（4）Standby modified, high temperature resistant filler and the mixing of aforesaid propylene acid esters pressure-sensitive adhesive emulsion
Grinding, discharging, produces high temperature resistant pressure sensitive adhesive.
Step（1）Described in sodium silicate solution and sodium chloride solution volume ratio be 1:1, the quality point of sodium silicate solution
Number is 30%, and the mass fraction of sodium chloride solution is 40%, and the addition of hydrochloric acid is the 1/2 of sodium silicate solution volume, the matter of hydrochloric acid
It is 31% to measure fraction.
Step（2）Described in zeolite powder particle diameter be 200 mesh, the mass fraction of lithium metasilicate solution is 20%, zeolite powder
Mass ratio with lithium metasilicate solution is 1:2, the mass ratio of filter residue and gel-like product is 1:3, the mass fraction of sulfuric acid solution is
98%, the addition of sulfuric acid solution is the 5% of filter residue quality.
Step（3）Described in bacillus subtilis bacteria suspension concentration be 105Cfu/mL, sealing and fermenting temperature be 30~
40 DEG C, the sealing and fermenting time is 3~5 days.
Step（6）Described in oil bath pot temperature be 80~85 DEG C, the mass fraction of ammoniacal liquor is 25%.
Step（7）Described in emulsifier op-10, the mass ratio of modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion
For 1:2:50.
The beneficial effects of the invention are as follows：
（1）The Silica hydrogel containing abundant silicone hydroxyl is made by hydrochloric acid decomposition method first in the present invention, then with silicic acid salt treatment zeolite,
Zeolite surface is made catalyst with silicone hydroxyl, then with the concentrated sulfuric acid, be dehydrated the silicone hydroxyl of Silica hydrogel and zeolite surface
Condensation reaction, formed the great Si-O-Si keys of bond energy, due to Si-O-Si keys bond energy be more than general organic matter in C-C keys and
C-O keys, therefore with good heat-resisting quantity, with its as filler prepare pressure sensitive adhesive can effectively improve pressure sensitive adhesive high temperature it is steady
It is qualitative；
（2）The present invention also uses natural resin in the presence of microorganism to filler modified, increase filler surface natural resin particle
Quantity, improve the compatibility between high temperature resistant filler and acrylate, and the natural resin of these low melting points is running into high temperature
In the case of can melt in advance, absorb partial heat, further improve pressure sensitive adhesive heat-resisting quantity, pressure sensitive adhesive produced by the present invention
Pliability and high-temperature stability are splendid, have broad application prospects.
Embodiment
Measure that 300~400mL mass fractions are 30% sodium silicate solution and 300~400mL mass fractions are 40% sodium chloride
Solution is fitted into beaker, with glass bar stirring 20~30min of mixing, beaker is put into refrigerator, saltout 3~5h at 2~4 DEG C,
Wait end of saltouing, it is 31% hydrochloric acid to continue to add 150~200mL mass fractions into beaker, with magnetic stirring apparatus with 200~
300r/min rotating speed 2~3h of stirring reaction, are separated by filtration removal filtrate, obtain gel-like product；It is 1 in mass ratio:2 by 200
Purpose zeolite powder pours into is 20% lithium metasilicate solution equipped with mass fraction, and beaker is moved into sonic oscillation instrument, with 30~
40kHz frequency ultrasound 3~5h of oscillation treatment, after sonic oscillation processing terminates, is separated by filtration and obtains filter residue；It is 1 in mass ratio:
3 will be fitted into the three-necked flask with dropping funel and agitator after filter residue and gel-like product mixing, then pass through dropping funel
The mass fraction of filter residue quality 5% is added into flask for 98% sulfuric acid solution, three-necked flask is moved into water-bath after completion of dropping
In, 60~70 DEG C are heated to, starts agitator with 200~300r/min rotating speed 3~5h of stirring reaction, mistake after reaction terminates
Filter, isolated filter cake discharges after freeze-drying, produces self-control high temperature resistant filler；Weigh 50~60g beeswaxs, 20~30g peaches
Glue, 30~40g gum arabics, 70~80g rosin and 300~400g self-control high temperature resistant fillers pour into mixed grinding in ball mill
1~2h, then the material after grinding is transferred in fermentation tank, it is 10 that 400~500mL concentration is added into fermentation tank5Cfu/mL is withered
Careless bacillus bacteria suspension, after stirring, sealed fermenter, heat-preservation fermentation 3~5 days at 30~40 DEG C；Treat that fermentation is completed
Afterwards, tunning is taken out, is separated by filtration and obtains filter residue, first filter residue is put into high-temperature sterilization box, is sterilized at 110~120 DEG C
15~20min, then the filter residue after sterilizing is freeze-dried with vacuum freeze-drying machine, produce modified, high temperature resistant filler after drying；To band
Have and 0.3~0.5g lauryl sodium sulfate, 1.3~1.5g nonyls are added in the four-hole boiling flask of agitator, thermometer and dropping funel
Base phenol polyethenoxy ether and 50~100mL deionized waters, start after agitator stirs and add 30~35g acrylic acid second
Ester, 2.2~3.0g hydroxy-ethyl acrylates, 2.5~3.6g Isooctyl acrylate monomers and 1.5~2.0g methacrylic acids, flask is moved
Enter in 60~70 DEG C of water-baths, and nitrogen is passed through into four-hole boiling flask as protection gas, insulated and stirred using 5~10mL/min speed
30~40min, obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, 80~85 DEG C are heated to, then add to four-hole boiling flask
Enter and 0.6~1.2g potassium peroxydisulfates are added after 0.4~0.8g potassium peroxydisulfates, 10~15min of stirring reaction, continue insulation reaction 2
~4h, after question response terminates, obtains reaction product, is that 25% ammoniacal liquor adjusts reactant pH to 7.0~8.0 with mass fraction, produces
Acrylate pressure-sensitive adhesive emulsion；It is 1 in mass ratio:2:50 by emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure sensitive
Latex solution is fitted into colloid mill, and with 1000~1200r/min rotating speed 1~2h of mixed grinding, discharging produces high temperature resistant pressure sensitive adhesive.
Example 1
Measure that 300mL mass fractions are 30% sodium silicate solution and 300mL mass fractions are that 40% sodium chloride solution is fitted into beaker,
With glass bar stirring mixing 20min, beaker is put into refrigerator, saltout 3h at 2 DEG C, waits end of saltouing, continues to add into beaker
Enter 150mL mass fractions for 31% hydrochloric acid, with magnetic stirring apparatus with 200r/min rotating speed stirring reaction 2h, be separated by filtration removal filter
Liquid, obtains gel-like product；It is 1 in mass ratio:2 by the zeolite powder of 200 mesh pour into equipped with mass fraction be 20% lithium metasilicate it is molten
In liquid, beaker is moved into sonic oscillation instrument, with 30kHz frequency ultrasound oscillation treatment 3h, after sonic oscillation processing terminates, filtering
Isolated filter residue；It is 1 in mass ratio:3 filter residue and gel-like product are mixed after load with dropping funel and agitator
In three-necked flask, then it is 98% sulfuric acid solution that the mass fraction of filter residue quality 5% is added by dropping funel into flask, is dripped
Three-necked flask is moved into water-bath after finishing, 60 DEG C are heated to, starts agitator with 200r/min rotating speed stirring reaction 3h,
Reaction is filtered after terminating, isolated filter cake, is discharged after freeze-drying, produces self-control high temperature resistant filler；Weigh 50g beeswaxs, 20g
Peach gum, 30g gum arabics, 70g rosin and 300g self-control high temperature resistant fillers pour into mixed grinding 1h in ball mill, then will grinding
Material afterwards is transferred in fermentation tank, and it is 10 that 400mL concentration is added into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, are stirred
After mixing uniformly, sealed fermenter, heat-preservation fermentation 3 days at 30 DEG C；Wait after the completion of fermenting, take out tunning, be separated by filtration
To filter residue, first filter residue is put into high-temperature sterilization box, sterilize 15min at 110 DEG C, then by the filter residue vacuum freeze-drying after sterilizing
Machine is freeze-dried, and modified, high temperature resistant filler is produced after drying；Into the four-hole boiling flask with agitator, thermometer and dropping funel
0.3g lauryl sodium sulfate, 1.3g NPEs and 50mL deionized waters are added, starts agitator and stirs
After add 30g ethyl acrylates, 2.2g hydroxy-ethyl acrylates, 2.5g Isooctyl acrylate monomers and 1.5g methacrylic acids, will burn
Bottle is moved into 60 DEG C of water-baths, and nitrogen is passed through into four-hole boiling flask as protection gas, insulated and stirred using 5mL/min speed
30min, obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, 80 DEG C are heated to, then 0.4g mistakes are added to four-hole boiling flask
0.6g potassium peroxydisulfates are added after potassium sulfate, stirring reaction 10min, continues insulation reaction 2h, after question response terminates, is reacted
Product, is that 25% ammoniacal liquor adjusts reactant pH to 7.0 with mass fraction, produces Acrylate pressure-sensitive adhesive emulsion；It is 1 in mass ratio:
2:50 are fitted into emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion in colloid mill, with 1000r/min
Rotating speed mixed grinding 1h, discharging, produces high temperature resistant pressure sensitive adhesive.
By high temperature resistant pressure sensitive adhesive produced by the present invention in being incubated 40min at 90 DEG C, pressure-sensitive adhesive emulsion is made, then gained is pressed
Quick latex solution, which is placed in coating machine, to be coated, and it is 140 DEG C to control gluing temperature, and rubberization thickness is 0.2mm, and the bonding time is
20s, is made pressure sensitive adhesive tape.
Example 2
Measure that 350mL mass fractions are 30% sodium silicate solution and 350mL mass fractions are that 40% sodium chloride solution is fitted into beaker,
With glass bar stirring mixing 25min, beaker is put into refrigerator, saltout 4h at 3 DEG C, waits end of saltouing, continues to add into beaker
Enter 180mL mass fractions for 31% hydrochloric acid, with magnetic stirring apparatus with 250r/min rotating speed stirring reaction 3h, be separated by filtration removal filter
Liquid, obtains gel-like product；It is 1 in mass ratio:2 by the zeolite powder of 200 mesh pour into equipped with mass fraction be 20% lithium metasilicate it is molten
In liquid, beaker is moved into sonic oscillation instrument, with 35kHz frequency ultrasound oscillation treatment 4h, after sonic oscillation processing terminates, filtering
Isolated filter residue；It is 1 in mass ratio:3 filter residue and gel-like product are mixed after load with dropping funel and agitator
In three-necked flask, then it is 98% sulfuric acid solution that the mass fraction of filter residue quality 5% is added by dropping funel into flask, is dripped
Three-necked flask is moved into water-bath after finishing, 65 DEG C are heated to, starts agitator with 250r/min rotating speed stirring reaction 4h,
Reaction is filtered after terminating, isolated filter cake, is discharged after freeze-drying, produces self-control high temperature resistant filler；Weigh 55g beeswaxs, 25g
Peach gum, 35g gum arabics, 75g rosin and 350g self-control high temperature resistant fillers pour into mixed grinding 2h in ball mill, then will grinding
Material afterwards is transferred in fermentation tank, and it is 10 that 450mL concentration is added into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, are stirred
After mixing uniformly, sealed fermenter, heat-preservation fermentation 4 days at 35 DEG C；Wait after the completion of fermenting, take out tunning, be separated by filtration
To filter residue, first filter residue is put into high-temperature sterilization box, sterilize 18min at 115 DEG C, then by the filter residue vacuum freeze-drying after sterilizing
Machine is freeze-dried, and modified, high temperature resistant filler is produced after drying；Into the four-hole boiling flask with agitator, thermometer and dropping funel
0.4g lauryl sodium sulfate, 1.4g NPEs and 80mL deionized waters are added, starts agitator and stirs
After add 33g ethyl acrylates, 2.6g hydroxy-ethyl acrylates, 3.1g Isooctyl acrylate monomers and 1.8g methacrylic acids, will burn
Bottle is moved into 65 DEG C of water-baths, and nitrogen is passed through into four-hole boiling flask as protection gas, insulated and stirred using 8mL/min speed
35min, obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, 83 DEG C are heated to, then 0.6g mistakes are added to four-hole boiling flask
0.9g potassium peroxydisulfates are added after potassium sulfate, stirring reaction 13min, continues insulation reaction 3h, after question response terminates, is reacted
Product, is that 25% ammoniacal liquor adjusts reactant pH to 7.5 with mass fraction, produces Acrylate pressure-sensitive adhesive emulsion；It is 1 in mass ratio:
2:50 are fitted into emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion in colloid mill, with 1100r/min
Rotating speed mixed grinding 2h, discharging, produces high temperature resistant pressure sensitive adhesive.
By high temperature resistant pressure sensitive adhesive produced by the present invention in being incubated 50min at 95 DEG C, pressure-sensitive adhesive emulsion is made, then gained is pressed
Quick latex solution is placed in being coated in coating machine, and it is 142 DEG C to control gluing temperature, and rubberization thickness is 0.2mm, and the bonding time is
21s, is made pressure sensitive adhesive tape.
Example 3
Measure that 400mL mass fractions are 30% sodium silicate solution and 400mL mass fractions are that 40% sodium chloride solution is fitted into beaker,
With glass bar stirring mixing 30min, beaker is put into refrigerator, saltout 5h at 4 DEG C, waits end of saltouing, continues to add into beaker
Enter 200mL mass fractions for 31% hydrochloric acid, with magnetic stirring apparatus with 300r/min rotating speed stirring reaction 3h, be separated by filtration removal filter
Liquid, obtains gel-like product；It is 1 in mass ratio:2 by the zeolite powder of 200 mesh pour into equipped with mass fraction be 20% lithium metasilicate it is molten
In liquid, beaker is moved into sonic oscillation instrument, with 40kHz frequency ultrasound oscillation treatment 5h, after sonic oscillation processing terminates, filtering
Isolated filter residue；It is 1 in mass ratio:3 filter residue and gel-like product are mixed after load with dropping funel and agitator
In three-necked flask, then it is 98% sulfuric acid solution that the mass fraction of filter residue quality 5% is added by dropping funel into flask, is dripped
Three-necked flask is moved into water-bath after finishing, 70 DEG C are heated to, starts agitator with 300r/min rotating speed stirring reaction 5h,
Reaction is filtered after terminating, isolated filter cake, is discharged after freeze-drying, produces self-control high temperature resistant filler；Weigh 60g beeswaxs, 30g
Peach gum, 40g gum arabics, 80g rosin and 400g self-control high temperature resistant fillers pour into mixed grinding 2h in ball mill, then will grinding
Material afterwards is transferred in fermentation tank, and it is 10 that 500mL concentration is added into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, are stirred
After mixing uniformly, sealed fermenter, heat-preservation fermentation 5 days at 40 DEG C；Wait after the completion of fermenting, take out tunning, be separated by filtration
To filter residue, first filter residue is put into high-temperature sterilization box, sterilize 20min at 120 DEG C, then by the filter residue vacuum freeze-drying after sterilizing
Machine is freeze-dried, and modified, high temperature resistant filler is produced after drying；Into the four-hole boiling flask with agitator, thermometer and dropping funel
0.5g lauryl sodium sulfate, 1.5g NPEs and 100mL deionized waters are added, starts agitator and stirs
After add 35g ethyl acrylates, 3.0g hydroxy-ethyl acrylates, 3.6g Isooctyl acrylate monomers and 2.0g methacrylic acids, will burn
Bottle is moved into 70 DEG C of water-baths, and nitrogen is passed through into four-hole boiling flask as protection gas, insulated and stirred using 10mL/min speed
40min, obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, 85 DEG C are heated to, then 0.8g mistakes are added to four-hole boiling flask
1.2g potassium peroxydisulfates are added after potassium sulfate, stirring reaction 15min, continues insulation reaction 4h, after question response terminates, is reacted
Product, is that 25% ammoniacal liquor adjusts reactant pH to 8.0 with mass fraction, produces Acrylate pressure-sensitive adhesive emulsion；It is 1 in mass ratio:
2:50 are fitted into emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion in colloid mill, with 1200r/min
Rotating speed mixed grinding 2h, discharging, produces high temperature resistant pressure sensitive adhesive.
By high temperature resistant pressure sensitive adhesive produced by the present invention in being incubated 60min at 100 DEG C, pressure-sensitive adhesive emulsion is made, then by gained
Pressure-sensitive adhesive emulsion is placed in coating machine and is coated, and it is 143 DEG C to control gluing temperature, and rubberization thickness is 0.3mm, and the bonding time is
21s, is made pressure sensitive adhesive tape.
High temperature resistant pressure sensitive adhesive obtained by the present embodiment is detected with waterborne polyurethane pressure-sensitive adhesives, as a result as shown in Table 1.
Detecting instrument is：Viscosity is held with sticky analyzer measure is held, viscosity tester determines viscosity.
Table one：
As seen from the above table, high temperature resistant pressure sensitive adhesive high-temperature stability of the present invention is good, hold viscous 30 under conditions of 175~180 DEG C~
33min not degummings, viscosity is 2550~2620mPas.
Claims (6)
1. a kind of preparation method of high temperature resistant pressure sensitive adhesive, it is characterised in that specifically preparation process is：
（1）Sodium silicate solution and sodium chloride solution are fitted into beaker, beaker refrigerator is put into after stirring mixing, at 2~4 DEG C
Saltout 3~5h, waits end of saltouing, and continues to add hydrochloric acid into beaker, 2~3h of stirring reaction, is separated by filtration removal filtrate, obtains
Gel-like product；
（2）Zeolite powder is poured into lithium metasilicate solution, sonic oscillation processing is filtrated to get filter residue, by filter residue and above-mentioned gel
It is fitted into after the mixing of shape product in three-necked flask, then is added dropwise into flask after sulfuric acid solution, completion of dropping in immigration water-bath, heating
60~70 DEG C are warming up to, 3~5h of stirring reaction, reaction is filtered after terminating, isolated filter cake discharges after freeze-drying, produced
Make high temperature resistant filler by oneself；
（3）Count by weight, weigh 50~60 parts of beeswaxs, 20~30 parts of peach gums, 30~40 parts of gum arabics, 70~80 parts
Rosin and 300~400 parts of above-mentioned self-control high temperature resistant filler mixed grindings, then the material after grinding is transferred in fermentation tank, Xiang Fa
Bacillus subtilis bacteria suspension, after stirring, sealing and fermenting are added in fermentation tank；
（4）Treat after the completion of above-mentioned fermentation, be filtrated to get filter residue, be freeze-dried after filter residue is sterilized, obtain modified, high temperature resistant filler, it is standby
With；
（5）Weigh 0.3~0.5g lauryl sodium sulfate, 1.3~1.5g NPEs add 50~100mL go from
In sub- water, 30~35g ethyl acrylates, 2.2~3.0g hydroxy-ethyl acrylates, 2.5~3.6g propylene are added after stirring
The different monooctyl ester of acid and 1.5~2.0g methacrylic acids, addition are warming up to 60~70 DEG C, under nitrogen protection, insulated and stirred after finishing
30~40min, obtains pre-emulsion；
（6）0.6~1.2g is added after adding 0.4~0.8g potassium peroxydisulfates, 10~15min of stirring reaction into above-mentioned pre-emulsion
Potassium peroxydisulfate, continues 2~4h of insulation reaction, after question response terminates, obtains reaction product, and reactant pH to 7.0 is adjusted with ammoniacal liquor
~8.0, produce Acrylate pressure-sensitive adhesive emulsion；
（7）By emulsifier op-10, step（4）Standby modified, high temperature resistant filler and the mixing of aforesaid propylene acid esters pressure-sensitive adhesive emulsion
Grinding, discharging, produces high temperature resistant pressure sensitive adhesive.
2. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that：Step（1）Described in
Sodium silicate solution and sodium chloride solution volume ratio be 1:1, the mass fraction of sodium silicate solution is 30%, sodium chloride solution
Mass fraction is 40%, and the addition of hydrochloric acid is the 1/2 of sodium silicate solution volume, and the mass fraction of hydrochloric acid is 31%.
3. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that：Step（2）Described in
Zeolite powder particle diameter be 200 mesh, the mass fraction of lithium metasilicate solution is 20%, the mass ratio of zeolite powder and lithium metasilicate solution
For 1:2, the mass ratio of filter residue and gel-like product is 1:3, the mass fraction of sulfuric acid solution is 98%, the addition of sulfuric acid solution
For the 5% of filter residue quality.
4. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that：Step（3）Described in
Bacillus subtilis bacteria suspension concentration be 105Cfu/mL, sealing and fermenting temperature is 30~40 DEG C, and the sealing and fermenting time is 3
~5 days.
5. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that：Step（6）Described in
Oil bath pot temperature be 80~85 DEG C, the mass fraction of ammoniacal liquor is 25%.
6. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that：Step（7）Described in
Emulsifier op-10, the mass ratio of modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion be 1:2:50.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107417170A (en) * | 2017-06-30 | 2017-12-01 | 常州瑞坦商贸有限公司 | A kind of anti-aging resin anchoring agent of high temperature resistant |
| CN108892909A (en) * | 2018-07-25 | 2018-11-27 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of high-strength hot stable type acrylate |
| CN109096947A (en) * | 2018-08-17 | 2018-12-28 | 佛山市森昂生物科技有限公司 | A kind of pressure sensitive adhesive |
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| US4831077A (en) * | 1984-12-20 | 1989-05-16 | Wacker-Chemie Gmbh | Novel-heat resistant adhesives |
| CN102533174A (en) * | 2011-12-07 | 2012-07-04 | 新丰杰力电工材料有限公司 | Emulsion type acrylate pressure sensitive adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4831077A (en) * | 1984-12-20 | 1989-05-16 | Wacker-Chemie Gmbh | Novel-heat resistant adhesives |
| CN102533174A (en) * | 2011-12-07 | 2012-07-04 | 新丰杰力电工材料有限公司 | Emulsion type acrylate pressure sensitive adhesive and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417170A (en) * | 2017-06-30 | 2017-12-01 | 常州瑞坦商贸有限公司 | A kind of anti-aging resin anchoring agent of high temperature resistant |
| CN108892909A (en) * | 2018-07-25 | 2018-11-27 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of high-strength hot stable type acrylate |
| CN109096947A (en) * | 2018-08-17 | 2018-12-28 | 佛山市森昂生物科技有限公司 | A kind of pressure sensitive adhesive |
| CN109096947B (en) * | 2018-08-17 | 2019-12-17 | 深圳市昌元兴科技有限公司 | Pressure-sensitive adhesive |
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