CN107236490B - 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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- CN107236490B CN107236490B CN201710510242.9A CN201710510242A CN107236490B CN 107236490 B CN107236490 B CN 107236490B CN 201710510242 A CN201710510242 A CN 201710510242A CN 107236490 B CN107236490 B CN 107236490B
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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 methods 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, make zeolite surface with silicone hydroxyl, make catalyst with the concentrated sulfuric acid again, make the silicone hydroxyl of Silica hydrogel and zeolite surface that dehydration condensation occur, form the great Si-O-Si key of bond energy, the C-C key and C-O key being greater than in general organic matter due to the bond energy of Si-O-Si key, with good heat-resisting quantity, use natural resin under the action 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 melt in advance in the case where encountering high temperature, absorb partial heat, further increase the heat-resisting quantity of pressure sensitive adhesive, pressure sensitive adhesive flexibility is made in the present invention and high-temperature stability is splendid , have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high temperature resistant pressure sensitive adhesive, belong to technical field of adhesive preparation.
Background technique
Pressure sensitive adhesive full name is pressure-sensitive adhesive, and abbreviation pressure sensitive adhesive is also commonly called as not doing due to being not easy solid feature
Glue.Pressure sensitive adhesive is one of current most widely used, maximum adhesive kind of yield, with daily life relationship is close can not
Point.It is a kind of during the bonding process to pressure-sensitive adhesive, in the case where lesser pressure acts on, does not need heating or molten
The effect of agent is just capable of forming firm bonding.Pressure sensitive adhesive and bonded object surface rely primarily on Van der Waals force carry out it is be bonded, because
This is with several big obvious advantages: (1) bonding process is easy；(2) it peels and is also easy to；(3) removing will not destroy gluing of surfaces
Structure；(4) glue-line is stablized, and the bonding time is long.
Pressure sensitive adhesive type is more, and pressure sensitive adhesive product is segmented into multiple types according to different classification standards.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..Since acrylate pressure-sensitive adhesive is fast light, ageing-resistant and water resistance is preferable, and with excellent pressure-sensitive
Property and adhesiveness, performance stablize, be widely used in many fields such as building, electric appliance, traffic, medical treatment, packaging, health,
Therefore become the main hot spot of pressure sensitive adhesive research field in recent years.
But acrylate pressure-sensitive adhesive high-temperature stability is generally all poor, and is difficult to be bonded low energy surface material,
Degumming phenomenon is easily generated 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 Diacetone Acrylamide/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
High temperature resistance hold the poor problem of viscosity but there is also degumming easy under hot environment.Because of a kind of high temperature resistant type third of the invention
Olefin(e) acid ester pressure-sensitive has positive meaning to pressure sensitive adhesive preparation technical field.
Summary of the invention
Present invention mainly solves the technical issues of, it is although fast light for current acrylate pressure-sensitive adhesive, resistance to ag(e)ing is good, but
It is that high-temperature stability is generally all poor, and is difficult to be bonded low energy surface material, under the hot environment more than 150 DEG C easily
The defect for generating degumming phenomenon, provides a kind of preparation method of high temperature resistant pressure sensitive adhesive.
In order to solve the above technical problems, the present invention is using technical solution as described below:
(1) sodium silicate solution and sodium chloride solution are fitted into beaker, beaker is put into refrigerator after being stirred, 2~4
Saltout 3~5h at DEG C, to the end of saltouing, continues that hydrochloric acid is added into beaker, is stirred to react 2~3h, is separated by filtration removal filtrate,
Obtain gel-like product；
(2) zeolite powder is poured into lithium metasilicate solution, filter residue is obtained by filtration, by filter residue and above-mentioned in sonic oscillation processing
It is fitted into three-necked flask after gel-like product mixing, then sulfuric acid solution is added dropwise into flask, moved into water-bath after being added dropwise,
60~70 DEG C are heated to, 3~5h is stirred to react, filters after reaction, isolated filter cake discharges after freeze-drying,
Up to self-control high temperature resistant filler；
(3) weigh 50~60g beeswax, 20~30g peach gum, 30~40g gum arabic, 70~80g rosin and 300~
The above-mentioned self-control high temperature resistant filler mixed grinding of 400g, then the material after grinding is transferred in fermentor, it is added into fermentor withered
Careless bacillus bacteria suspension is sealed by fermentation after mixing evenly；
(4) filter residue is obtained by filtration after fermentation to above-mentioned, first by the 15~20min that sterilizes at 110~120 DEG C of filter residue, then
Freeze-drying, obtains modified, high temperature resistant filler, spare；
(5) 0.3~0.5g lauryl sodium sulfate, 1.3~1.5g nonylphenol polyoxyethylene ether are added into four-hole boiling flask
With 50~100mL deionized water, add after mixing evenly 30~35g ethyl acrylate, 2.2~3.0g hydroxy-ethyl acrylate,
2.5~3.6g Isooctyl acrylate monomer and 1.5~2.0g methacrylic acid move into four-hole boiling flask in 60~70 DEG C of water-baths,
Under nitrogen protection, 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 peroxydisulfate, stirring is added to four-hole boiling flask
0.6~1.2g potassium peroxydisulfate is added after 10~15min of reaction, continues 2~4h of insulation reaction, it is anti-to after reaction, obtain
Product is answered, adjusts reactant pH to 7.0~8.0 with ammonium hydroxide to get Acrylate pressure-sensitive adhesive emulsion；
(7) by emulsifier op-10, the spare modified, high temperature resistant filler of step (4) and above-mentioned Acrylate pressure-sensitive adhesive emulsion
Mixed grinding discharges to get high temperature resistant pressure sensitive adhesive.
The volume ratio of sodium silicate solution and sodium chloride solution as described in step (1) is 1:1, the quality point of sodium silicate solution
Number is 30%, and the mass fraction of sodium chloride solution is 40%, and the additional amount of hydrochloric acid is the 1/2 of sodium silicate solution volume, the matter of hydrochloric acid
Measuring score is 31%.
Zeolite powder partial size described in step (2) is 200 mesh, and the mass fraction of lithium metasilicate solution is 20%, zeolite powder
It is 1:2 with the mass ratio of lithium metasilicate solution, the mass ratio of filter residue and gel-like product is 1:3, and the mass fraction of sulfuric acid solution is
98%, the additional amount of sulfuric acid solution is the 5% of filter residue quality.
The concentration of bacillus subtilis bacteria suspension described in step (3) is 105Cfu/mL, be sealed by fermentation temperature be 30~
40 DEG C, being sealed by fermentation the time is 3~5 days.
Oil bath pot temperature described in step (6) is 80~85 DEG C, and the mass fraction of ammonium hydroxide is 25%.
The mass ratio of emulsifier op-10 described in step (7), modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion
For 1:2:50.
The beneficial effects of the present invention are:
(1) 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 makes zeolite surface with silicone hydroxyl, then makees catalyst with the concentrated sulfuric acid, and the silicone hydroxyl of Silica hydrogel and zeolite surface occurs
Dehydration condensation forms the great Si-O-Si key of bond energy, the C-C being greater than in general organic matter due to the bond energy of Si-O-Si key
Key and C-O key, therefore there is good heat-resisting quantity, using it to prepare pressure sensitive adhesive as filler can effectively improve the height of pressure sensitive adhesive
Temperature stability；
(2) present invention also uses natural resin under the action of microorganism to filler modified, increase filler surface natural resin
The quantity of particle improves the compatibility between high temperature resistant filler and acrylate, and the natural resin of these low melting points is encountering
It can be melted in advance in the case where high temperature, absorb partial heat, further increase the heat-resisting quantity of pressure sensitive adhesive, pressure produced by the present invention
Quick glue flexibility and high-temperature stability are splendid, have broad application prospects.
Specific embodiment
Measurement 300~400mL mass fraction is 30% sodium silicate solution and 300~400mL mass fraction is 40% sodium chloride
Solution is fitted into beaker, is stirred 20~30min with glass bar, and beaker is put into refrigerator, and saltout 3~5h at 2~4 DEG C,
To the end of saltouing, continue that 150~200mL mass fraction is added into beaker to be 31% hydrochloric acid, with magnetic stirring apparatus with 200~
300r/min revolving speed is stirred to react 2~3h, is separated by filtration removal filtrate, obtains gel-like product；It is in mass ratio 1:2 by 200
It is that beaker is moved into sonic oscillation instrument in 20% lithium metasilicate solution that purpose zeolite powder, which is poured into equipped with mass fraction, with 30~
Frequency ultrasound 3~5h of oscillation treatment of 40kHz, sonic oscillation after treatment are separated by filtration to obtain filter residue；In mass ratio it is 1:
3 will be fitted into the three-necked flask with dropping funel and blender after filter residue and gel-like product mixing, then pass through dropping funel
The mass fraction that filter residue quality 5% is added into flask is 98% sulfuric acid solution, and three-necked flask is moved into water-bath after being added dropwise
In, 60~70 DEG C are heated to, starts blender with 200~300r/min revolving speed and is stirred to react 3~5h, after reaction mistake
Filter, isolated filter cake are discharged after freeze-drying to get self-control high temperature resistant filler；Weigh 50~60g beeswax, 20~30g peach
Glue, 30~40g gum arabic, 70~80g rosin and 300~400g self-control high temperature resistant filler pour into mixed grinding in ball mill
1~2h, then the material after grinding is transferred in fermentor, it is 10 that 400~500mL concentration is added into fermentor5Cfu/mL is withered
Careless bacillus bacteria suspension, after mixing evenly, sealed fermenter, heat-preservation fermentation 3~5 days at 30~40 DEG C；It is completed wait ferment
Afterwards, tunning is taken out, is separated by filtration to obtain filter residue, first filter residue is put into high-temperature sterilization box, sterilize at 110~120 DEG C
15~20min, then the filter residue after sterilizing is freeze-dried with vacuum freeze-drying machine, up to modified, high temperature resistant filler after drying；To band
There is addition 0.3~0.5g lauryl sodium sulfate, 1.3~1.5g nonyl in the four-hole boiling flask of blender, thermometer and dropping funel
Base phenol polyethenoxy ether and 50~100mL deionized water, starting blender add 30~35g acrylic acid second after mixing evenly
Ester, 2.2~3.0g hydroxy-ethyl acrylate, 2.5~3.6g Isooctyl acrylate monomer and 1.5~2.0g methacrylic acid, 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 rate
30~40min obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, is heated to 80~85 DEG C, then add to four-hole boiling flask
Enter 0.4~0.8g potassium peroxydisulfate, adds 0.6~1.2g potassium peroxydisulfate after being stirred to react 10~15min, continue insulation reaction 2
~4h, to after reaction, obtain reaction product, with mass fraction be 25% ammonium hydroxide adjust reactant pH to 7.0~8.0 to get
Acrylate pressure-sensitive adhesive emulsion；It is in mass ratio 1:2:50 by emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure sensitive
Latex solution is fitted into colloid mill, with 1000~1200r/min revolving speed 1~2h of mixed grinding, is discharged to get high temperature resistant pressure sensitive adhesive.
Example 1
Measurement 300mL mass fraction is 30% sodium silicate solution and 300mL mass fraction is that 40% sodium chloride solution is packed into burning
In cup, it is stirred 20min with glass bar, beaker is put into refrigerator, saltout 3h at 2 DEG C, to the end of saltouing, continues to beaker
Middle addition 150mL mass fraction is 31% hydrochloric acid, is stirred to react 2h with magnetic stirring apparatus with 200r/min revolving speed, is separated by filtration
Except filtrate, gel-like product is obtained；It is in mass ratio that 1:2 pours into the zeolite powder of 200 mesh equipped with mass fraction is 20% silicic acid
In lithium solution, beaker is moved into sonic oscillation instrument, with the frequency ultrasound oscillation treatment 3h of 30kHz, sonic oscillation after treatment,
It is separated by filtration to obtain filter residue；It is packed into after in mass ratio mixing filter residue and gel-like product for 1:3 and has dropping funel and stirring
In the three-necked flask of device, then passing through dropping funel the mass fraction of filter residue quality 5% is added into flask is 98% sulfuric acid solution, drop
Three-necked flask is moved into water-bath after adding, is heated to 60 DEG C, it is anti-with the stirring of 200r/min revolving speed to start blender
3h is answered, is filtered after reaction, isolated filter cake is discharged after freeze-drying to get self-control high temperature resistant filler；Weigh 50g bee
Wax, 20g peach gum, 30g gum arabic, 70g rosin and 300g self-control high temperature resistant filler pour into mixed grinding 1h in ball mill, then
Material after grinding is transferred in fermentor, it is 10 that 400mL concentration is added into fermentor5Cfu/mL bacillus subtilis bacterium is outstanding
Liquid, after mixing evenly, sealed fermenter, heat-preservation fermentation 3 days at 30 DEG C；To after fermentation, take out tunning, filtering point
From filter residue is obtained, first filter residue is put into high-temperature sterilization box, sterilize 15min at 110 DEG C, then by the filter residue vacuum after sterilizing
Freeze dryer freeze-drying, up to modified, high temperature resistant filler after drying；To four mouthfuls of burnings with blender, thermometer and dropping funel
0.3g lauryl sodium sulfate, 1.3g nonylphenol polyoxyethylene ether and 50mL deionized water, starting blender stirring are added in bottle
30g ethyl acrylate, 2.2g hydroxy-ethyl acrylate, 2.5g Isooctyl acrylate monomer and 1.5g methacrylic acid are added after uniformly,
Flask 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 rate
30min obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, is heated to 80 DEG C, then 0.4g mistake is added to four-hole boiling flask
Potassium sulfate adds 0.6g potassium peroxydisulfate after being stirred to react 10min, continues insulation reaction 2h, to after reaction, be reacted
Product is that 25% ammonium hydroxide adjusts reactant pH to 7.0 to get Acrylate pressure-sensitive adhesive emulsion with mass fraction；In mass ratio it is 1:
Emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion are fitted into colloid mill by 2:50, with 1000r/min
Revolving speed mixed grinding 1h discharges to get high temperature resistant pressure sensitive adhesive.
High temperature resistant pressure sensitive adhesive produced by the present invention is kept the temperature into 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, control gluing temperature be 140 DEG C, rubberization thickness 0.2mm, bonding the time be
Pressure sensitive adhesive tape is made in 20s.
Example 2
Measurement 350mL mass fraction is 30% sodium silicate solution and 350mL mass fraction is that 40% sodium chloride solution is packed into burning
In cup, it is stirred 25min with glass bar, beaker is put into refrigerator, saltout 4h at 3 DEG C, to the end of saltouing, continues to beaker
Middle addition 180mL mass fraction is 31% hydrochloric acid, is stirred to react 3h with magnetic stirring apparatus with 250r/min revolving speed, is separated by filtration
Except filtrate, gel-like product is obtained；It is in mass ratio that 1:2 pours into the zeolite powder of 200 mesh equipped with mass fraction is 20% silicic acid
In lithium solution, beaker is moved into sonic oscillation instrument, with the frequency ultrasound oscillation treatment 4h of 35kHz, sonic oscillation after treatment,
It is separated by filtration to obtain filter residue；It is packed into after in mass ratio mixing filter residue and gel-like product for 1:3 and has dropping funel and stirring
In the three-necked flask of device, then passing through dropping funel the mass fraction of filter residue quality 5% is added into flask is 98% sulfuric acid solution, drop
Three-necked flask is moved into water-bath after adding, is heated to 65 DEG C, it is anti-with the stirring of 250r/min revolving speed to start blender
4h is answered, is filtered after reaction, isolated filter cake is discharged after freeze-drying to get self-control high temperature resistant filler；Weigh 55g bee
Wax, 25g peach gum, 35g gum arabic, 75g rosin and 350g self-control high temperature resistant filler pour into mixed grinding 2h in ball mill, then
Material after grinding is transferred in fermentor, it is 10 that 450mL concentration is added into fermentor5Cfu/mL bacillus subtilis bacterium is outstanding
Liquid, after mixing evenly, sealed fermenter, heat-preservation fermentation 4 days at 35 DEG C；To after fermentation, take out tunning, filtering point
From filter residue is obtained, first filter residue is put into high-temperature sterilization box, sterilize 18min at 115 DEG C, then by the filter residue vacuum after sterilizing
Freeze dryer freeze-drying, up to modified, high temperature resistant filler after drying；To four mouthfuls of burnings with blender, thermometer and dropping funel
0.4g lauryl sodium sulfate, 1.4g nonylphenol polyoxyethylene ether and 80mL deionized water, starting blender stirring are added in bottle
33g ethyl acrylate, 2.6g hydroxy-ethyl acrylate, 3.1g Isooctyl acrylate monomer and 1.8g methacrylic acid are added after uniformly,
Flask 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 rate
35min obtains pre-emulsion；Four-hole boiling flask is moved into oil bath pan, is heated to 83 DEG C, then 0.6g mistake is added to four-hole boiling flask
Potassium sulfate adds 0.9g potassium peroxydisulfate after being stirred to react 13min, continues insulation reaction 3h, to after reaction, be reacted
Product is that 25% ammonium hydroxide adjusts reactant pH to 7.5 to get Acrylate pressure-sensitive adhesive emulsion with mass fraction；In mass ratio it is 1:
Emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion are fitted into colloid mill by 2:50, with 1100r/min
Revolving speed mixed grinding 2h discharges to get high temperature resistant pressure sensitive adhesive.
High temperature resistant pressure sensitive adhesive produced by the present invention is kept the temperature into 50min at 95 DEG C, pressure-sensitive adhesive emulsion is made, then gained is pressed
Quick latex solution, which is placed in coating machine, to be coated, control gluing temperature be 142 DEG C, rubberization thickness 0.2mm, bonding the time be
Pressure sensitive adhesive tape is made in 21s.
Example 3
Measurement 400mL mass fraction is 30% sodium silicate solution and 400mL mass fraction is that 40% sodium chloride solution is packed into burning
In cup, it is stirred 30min with glass bar, beaker is put into refrigerator, saltout 5h at 4 DEG C, to the end of saltouing, continues to beaker
Middle addition 200mL mass fraction is 31% hydrochloric acid, is stirred to react 3h with magnetic stirring apparatus with 300r/min revolving speed, is separated by filtration
Except filtrate, gel-like product is obtained；It is in mass ratio that 1:2 pours into the zeolite powder of 200 mesh equipped with mass fraction is 20% silicic acid
In lithium solution, beaker is moved into sonic oscillation instrument, with the frequency ultrasound oscillation treatment 5h of 40kHz, sonic oscillation after treatment,
It is separated by filtration to obtain filter residue；It is packed into after in mass ratio mixing filter residue and gel-like product for 1:3 and has dropping funel and stirring
In the three-necked flask of device, then passing through dropping funel the mass fraction of filter residue quality 5% is added into flask is 98% sulfuric acid solution, drop
Three-necked flask is moved into water-bath after adding, is heated to 70 DEG C, it is anti-with the stirring of 300r/min revolving speed to start blender
5h is answered, is filtered after reaction, isolated filter cake is discharged after freeze-drying to get self-control high temperature resistant filler；Weigh 60g bee
Wax, 30g peach gum, 40g gum arabic, 80g rosin and 400g self-control high temperature resistant filler pour into mixed grinding 2h in ball mill, then
Material after grinding is transferred in fermentor, it is 10 that 500mL concentration is added into fermentor5Cfu/mL bacillus subtilis bacterium is outstanding
Liquid, after mixing evenly, sealed fermenter, heat-preservation fermentation 5 days at 40 DEG C；To after fermentation, take out tunning, filtering point
From filter residue is obtained, first filter residue is put into high-temperature sterilization box, sterilize 20min at 120 DEG C, then by the filter residue vacuum after sterilizing
Freeze dryer freeze-drying, up to modified, high temperature resistant filler after drying；To four mouthfuls of burnings with blender, thermometer and dropping funel
0.5g lauryl sodium sulfate, 1.5g nonylphenol polyoxyethylene ether and 100mL deionized water, starting blender stirring are added in bottle
35g ethyl acrylate, 3.0g hydroxy-ethyl acrylate, 3.6g Isooctyl acrylate monomer and 2.0g methacrylic acid are added after uniformly,
Flask is moved into 70 DEG C of water-baths, and nitrogen is passed through into four-hole boiling flask as protection gas using 10mL/min rate, heat preservation is stirred
40min is mixed, pre-emulsion is obtained；Four-hole boiling flask is moved into oil bath pan, is heated to 85 DEG C, then 0.8g is added to four-hole boiling flask
Potassium peroxydisulfate adds 1.2g potassium peroxydisulfate after being stirred to react 15min, continues insulation reaction 4h, anti-to after reaction, obtain
Product is answered, is that 25% ammonium hydroxide adjusts reactant pH to 8.0 to get Acrylate pressure-sensitive adhesive emulsion with mass fraction；It is in mass ratio
Emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion are fitted into colloid mill by 1:2:50, with 1200r/
Min revolving speed mixed grinding 2h discharges to get high temperature resistant pressure sensitive adhesive.
High temperature resistant pressure sensitive adhesive produced by the present invention is kept the temperature into 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, control gluing temperature be 143 DEG C, rubberization thickness 0.3mm, bonding the time be
Pressure sensitive adhesive tape is made in 21s.
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 are as follows: hold viscosity with sticky analyzer measurement is held, viscosity tester measures viscosity.
Table one:
As seen from the above table, high temperature resistant pressure sensitive adhesive high-temperature stability of the present invention is good, holds viscous 30 under conditions of 175~180 DEG C
~33min not degumming, viscosity are 2550~2620mPas.
Claims (6)
1. a kind of preparation method of high temperature resistant pressure sensitive adhesive, it is characterised in that specific preparation step are as follows:
(1) sodium silicate solution and sodium chloride solution are fitted into beaker, beaker is put into refrigerator after being stirred, at 2~4 DEG C
Saltout 3~5h, to the end of saltouing, continues that hydrochloric acid is added into beaker, is stirred to react 2~3h, is separated by filtration removal filtrate, obtains
Gel-like product；
(2) zeolite powder is poured into lithium metasilicate solution, filter residue is obtained by filtration, by filter residue and above-mentioned gel in sonic oscillation processing
It is fitted into three-necked flask after the mixing of shape product, then sulfuric acid solution is added dropwise into flask, moved into water-bath after being added dropwise, heating
Be warming up to 60~70 DEG C, be stirred to react 3~5h, filter after reaction, isolated filter cake, after freeze-drying discharge to get
Make high temperature resistant filler by oneself；
(3) according to parts by weight, 50~60 parts of beeswaxs, 20~30 parts of peach gums, 30~40 parts of gum arabics, 70~80 parts are weighed
Rosin and 300~400 parts of above-mentioned self-control high temperature resistant filler mixed grindings, then the material after grinding is transferred in fermentor, Xiang Fa
Bacillus subtilis bacteria suspension is added in fermentation tank, after mixing evenly, is sealed by fermentation；
(4) filter residue is obtained by filtration after fermentation to above-mentioned, is freeze-dried after filter residue is sterilized, obtain modified, high temperature resistant filler, it is standby
With；
(5) 0.3~0.5g lauryl sodium sulfate is added into four-hole boiling flask, 1.3~1.5g nonylphenol polyoxyethylene ether is added
In 50~100mL deionized water, add after mixing evenly 30~35g ethyl acrylate, 2.2~3.0g hydroxy-ethyl acrylate,
2.5~3.6g Isooctyl acrylate monomer and 1.5~2.0g methacrylic acid, are warming up to 60~70 DEG C after addition, protect 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 peroxydisulfate is added to four-hole boiling flask, be stirred to react
0.6~1.2g potassium peroxydisulfate is added after 10~15min, continues 2~4h of insulation reaction, is produced to after reaction, obtain reaction
Object adjusts reactant pH to 7.0~8.0 with ammonium hydroxide to get Acrylate pressure-sensitive adhesive emulsion；
(7) the spare modified, high temperature resistant filler of emulsifier op-10, step (4) and above-mentioned Acrylate pressure-sensitive adhesive emulsion are mixed
Grinding discharges to get 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: described in step (1)
Sodium silicate solution and the volume ratio of sodium chloride solution be 1:1, the mass fraction of sodium silicate solution is 30%, sodium chloride solution
Mass fraction is 40%, and the additional amount 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: described in step (2)
Zeolite powder partial size 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, and the mass fraction of sulfuric acid solution is 98%, the additional amount of sulfuric acid solution
It is 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: described in step (3)
Bacillus subtilis bacteria suspension concentration be 105Cfu/mL, being sealed by fermentation temperature is 30~40 DEG C, and being sealed by fermentation the 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: described in step (6)
Oil bath pot temperature be 80~85 DEG C, the mass fraction of ammonium hydroxide is 25%.
6. a kind of preparation method of high temperature resistant pressure sensitive adhesive according to claim 1, it is characterised in that: described in step (7)
Emulsifier op-10, modified, high temperature resistant filler and Acrylate pressure-sensitive adhesive emulsion mass ratio be 1:2:50.
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| CN109096947B (en) * | 2018-08-17 | 2019-12-17 | 深圳市昌元兴科技有限公司 | Pressure-sensitive adhesive |
Citations (2)
| 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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| 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 |
Non-Patent Citations (1)
| Title |
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| 耐高温压敏胶粘带的研究进展;李周 等;《粘接》;20051030;第26卷(第5期);第35-37页 |
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