CN107286889A - A kind of high temperature resistant environment-protective adhesive and preparation method thereof - Google Patents
A kind of high temperature resistant environment-protective adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN107286889A CN107286889A CN201710644697.XA CN201710644697A CN107286889A CN 107286889 A CN107286889 A CN 107286889A CN 201710644697 A CN201710644697 A CN 201710644697A CN 107286889 A CN107286889 A CN 107286889A
- Authority
- CN
- China
- Prior art keywords
- parts
- starch
- modified
- high temperature
- temperature resistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
- C08B31/185—Derivatives of oxidised starch, e.g. crosslinked oxidised starch
-
- 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
-
- 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
- C09J11/06—Non-macromolecular additives organic
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of high temperature resistant environment-protective adhesive and preparation method thereof, it is related to field of adhesive technology, includes the raw material of following part meter：45 ~ 55 parts of 65 ~ 70 parts of modifying epoxy resin by organosilicon, 55 ~ 65 parts of modified starch, 25 ~ 35 parts of filler, 10 ~ 15 parts of redispersible latex powder, 20 ~ 25 parts of auxiliary agent and water.The present invention be affected by temperature it is smaller, with good caking property, raw material safety and environmental protection.
Description
Technical field
The present invention relates to field of adhesive technology, and in particular to a kind of high temperature resistant environment-protective adhesive and preparation method thereof.
Background technology
At present, the adhesive of China is main using formaldehyde as main production raw material, i.e. urea-formaldehyde resin adhesive, phenolic resin glue and three
Melamine-formaldehyde resin glue, its yield accounts for more than the 90% of whole wood-based panel industry adhesive.But, the first discharged when using
Injury of the aldehyde to human body is bigger, and suction is likely to result in disease to people for a long time, causes irremediable loss, in addition, in the market is existing
Some floor glues have the following disadvantages：When being overheated by high temperature or weather, plybonding effect declines, cause floor covering layers to ftracture etc.
Problem.
The content of the invention
It is an object of the invention to provide a kind of high temperature resistant environment-protective adhesive and preparation method thereof, smaller, tool is affected by temperature
There are good caking property, raw material safety and environmental protection.
The invention provides following technical scheme：A kind of high temperature resistant environment-protective adhesive, includes the raw material of following part meter：Have
65 ~ 70 parts of machine silicon modified epoxy resin, 55 ~ 65 parts of modified starch, 25 ~ 35 parts of filler, 10 ~ 15 parts of redispersible latex powder,
45 ~ 55 parts of 20 ~ 25 parts of auxiliary agent and water；
The modifying epoxy resin by organosilicon includes the raw material that following part is counted：30 ~ 40 parts of bisphenol A epoxide resin, amido silicon oil 25 ~
27 parts and 16 ~ 18 parts of MDA；
The modified starch includes the raw material that following part is counted：14 ~ 16 parts of starch, 10 ~ 12 parts of amido silicon oil, modified alta-mud 8 ~ 10
10 ~ 20 parts of part, 5 ~ 7 parts of sodium ethylene diamine tetracetate, 1 ~ 3 part of sodium trimetaphosphate and water；
The auxiliary agent includes the raw material that following part is counted：6 ~ 8 parts of water-loss reducer, 4 ~ 6 parts of preservative, 4 ~ 6 parts of antifreezing agent, waterproofing agent 2 ~ 4
2 ~ 4 parts of part and colouring agent.
Wherein, the filler includes the raw material that following part is counted：8 ~ 11 parts of wax phase change microballoon, modified expansible graphite 5 ~ 7
3 ~ 5 parts of part, 5 ~ 7 parts of expanded perlite and talcum powder.
Wherein, the wax phase change microballoon is made up of the paraffin and Opacifying polymers shell enclosed, the paraffin encapsulation
In in polymer shell.
Wherein, the Opacifying polymers shell is hollow polymer spheroid, and the hollow polymer spheroid is acrylic acid
The polymer of ester and styrene composition.
Wherein, the modified expansible graphite includes the raw material that following part is counted：1 ~ 2 part of expansible graphite, polyvinyl alcohol 1 ~ 2
1 ~ 2 part of part, 0.8 ~ 1.2 part of boric acid aqueous solution, 0.4 ~ 0.6 part of ferrous sulfate and deionized water.
Wherein, the preparation method of the modified expansible graphite is：Polyvinyl alcohol is weighed according to proportioning, deionized water is added
In, 30 ~ 35min is heated under the conditions of 55 ~ 60 DEG C, stirring and dissolving obtains poly-vinyl alcohol solution to transparence；Weigh inflatable stone
Ink, is put into poly-vinyl alcohol solution, mixes 25 ~ 30min with 100 ~ 150r/min rotating speed, powder is obtained after drying process
Material, then adds to boric acid aqueous solution and ferrous sulfate, 10 ~ 15min of stirring reaction, filters, dry, and obtains modified inflatable stone
Ink.
Wherein, the method for preparing modified bentonite is：Bentonite is put into boric acid aqueous solution, with 100 ~ 400r/
Min rotating speed mixes 30 ~ 50min, filtering, and it is 7 to retain filter residue and be washed to pH value, after then filter residue is dried 100 ~
20 ~ 40min is calcined under the conditions of 300 DEG C and obtains the modified alta-mud.
Wherein, the water-loss reducer includes the raw material that following part is counted：1 ~ 2 part of cellulose ether, 1 ~ 2 part of polyvinyl alcohol and starch ether
0.4 ~ 0.6 part, the preservative be sodium tetraborate, sodium benzoate, natrium nitrosum, sodium sulfite and triethanolamine in one kind or
Several, the antifreezing agent is calcium chloride or ethylene glycol, and the waterproofing agent is waterproofing agent of organosilicon, nano waterproof agent and aluminium salt waterproof
One or more in agent, the colouring agent is any of titanium dioxide, carbon black, red titanium oxide, iron oxide yellow and barba hispanica.
Wherein, the Nano silica sol is dispersion liquid of the nanosized silica particles in water, nanometer grade silica
The mass fraction of particle is 40 ~ 50%, and the starch is the one of cornstarch, tapioca, farina and wheaten starch
Plant or several, the redispersible latex powder is vinylacetate and ethylene copolymer rubber powder.
The present invention provides a kind of preparation method of high temperature resistant environment-protective adhesive, comprises the following steps：
（1）, pretreatment of starch
Weigh starch to add in the water of 2 ~ 3 times of parts by weight, be warming up to 55 ~ 65 degrees Celsius, stirring obtains starch emulsion, then wherein
Addition accounts for the sodium hydroxide of starch quality 0.3 ~ 0.7%, and then 10 ~ 20min of stirring reaction adds and account for starch quality 1.5 ~ 2.5%
Potassium permanganate carry out first time oxidation, 10 ~ 15min of stirring reaction, then add account for starch quality 2.5 ~ 3% sulfuric acid carry out
Second aoxidizes, finally starch emulsion is carried out suction filtration, wash to it is neutral, dehydrate and obtain pretreated starch；
（2）, prepare modified starch
Weigh sodium ethylene diamine tetracetate and step（1）Pretreated starch, is added to the water and is heated under 60 ~ 80 degrees celsius
30 ~ 40min is dissolved, 10 ~ 25 degrees Celsius is cooled to and obtains starch milk；
Weigh modified alta-mud to add in foregoing obtained starch milk, add sodium trimetaphosphate, taken the photograph after being well mixed 50 ~ 70
20 ~ 25min is reacted under the conditions of family name's degree, amido silicon oil is then added, is well mixed, obtains modified starch slurry, then by washing,
It is dehydrated and dries, obtains the modified starch, it is standby；
（3）, prepare modifying epoxy resin by organosilicon
Amido silicon oil and bisphenol A epoxide resin are mixed, are dissolved in acetone, with 200 ~ 300r/min rotating speed stirring 25 ~
35min, is warming up to 120 ~ 150 degrees Celsius, reacts 50 ~ 60min, and after reaction terminates, vacuum distillation removes acetone, obtains mixture
Material, adds MDA mixing, 40 ~ 50min is stirred with 100 ~ 120r/min rotating speed, dry, after cooling thereto
The modifying epoxy resin by organosilicon is obtained, it is standby；
（4）, by step（2）Obtained modified starch and step（3）Obtained modifying epoxy resin by organosilicon mixing, is added remaining
Raw material, stirs 20 ~ 30min with 200 ~ 300r/min rotating speed, obtains the high temperature resistant environment-protective adhesive.
Beneficial effects of the present invention：Be affected by temperature it is smaller, with good caking property, raw material safety and environmental protection, specifically
It is as follows：
（1）, addition cellulose ether, polyvinyl alcohol and starch ether, as water-loss reducer, on the one hand can cause the present invention in the feed
The adhesive of the present invention has water-retaining property, on the other hand can also improve viscosity so that application property of the present invention is good and bonds strong
Degree is high, is affected by temperature smaller；
（2）, the present invention add modified expansible graphite in the feed, by more homogeneous and densification can be formed after high-temp combustion
Carbon-coating, enhance flameproof effect；Nano silica sol is added in the feed, water resistance and heat-resisting quantity is improved, and is significantly improved
The thixotropy of system；
（3）, the present invention in the feed add wax phase change microballoon, the paraffin of encapsulation is isolated with other raw materials, effectively protected
The chemical property of paraffin, flexible excellent, light weight, chemicals-resistant, low-permeable, good mechanical strength, when extraneous temperature
During degree rise, solid paraffin absorbs heat, is undergone phase transition after heat absorption enough, solid paraffin is converted into atoleine；When extraneous temperature
After degree reduction, atoleine release heat is undergone phase transition, atoleine is converted into solid after release enough, this heat absorption and is put
Hot merit energy, can make the temperature of wax phase change microsphere surface keep relative constancy within a certain period of time so that of the invention is gluing
Agent also has heat-insulating property；
（4）, the present invention add modifying epoxy resin by organosilicon in the feed, using amido silicon oil and MDA to double
Phenol A epoxy resin, which is modified, to be obtained, with good physical and chemical properties, with adhesion strength is high, dielectric properties are good,
Deformation retract rate is small, good stability of the dimension, and hardness is high and the features such as pliability, thus improve the ageing resistace of the present invention with
Caking ability；
（5）, each materials safety environmental protection in the present invention, it is formaldehydeless to wait pernicious gas to produce, improve environmental-protecting performance.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.
Embodiment 1
A kind of high temperature resistant environment-protective adhesive, includes the raw material of following part meter：65 parts of modifying epoxy resin by organosilicon, modified starch 55
Part, 25 parts of filler, 10 parts of redispersible latex powder, 20 parts of auxiliary agent and 45 parts of water；
The modifying epoxy resin by organosilicon includes the raw material that following part is counted：30 parts of bisphenol A epoxide resin, 25 parts of amido silicon oil and
16 parts of MDA；
The modified starch includes the raw material that following part is counted：14 parts of starch, 10 parts of amido silicon oil, 8 parts of modified alta-mud, ethylenediamine
10 parts of 5 parts of tetraacethyl sodium, 1 part of sodium trimetaphosphate and water；
The auxiliary agent includes the raw material that following part is counted：6 parts of water-loss reducer, 4 parts of preservative, 4 parts of antifreezing agent, 2 parts of waterproofing agent and coloring
2 parts of agent.
Wherein, the filler includes the raw material that following part is counted：It is 8 parts of wax phase change microballoon, modified 5 parts of expansible graphite, swollen
3 parts of 5 parts of swollen perlite and talcum powder.
Wherein, the wax phase change microballoon is made up of the paraffin and Opacifying polymers shell enclosed, the paraffin encapsulation
In in polymer shell.
Wherein, the Opacifying polymers shell is hollow polymer spheroid, and the hollow polymer spheroid is acrylic acid
The polymer of ester and styrene composition.
Wherein, the modified expansible graphite includes the raw material that following part is counted：1 part of expansible graphite, 1 part of polyvinyl alcohol,
1 part of 0.8 part of boric acid aqueous solution, 0.4 part of ferrous sulfate and deionized water.
Wherein, the preparation method of the modified expansible graphite is：Polyvinyl alcohol is weighed according to proportioning, deionized water is added
In, 30min is heated under the conditions of 55 DEG C, stirring and dissolving obtains poly-vinyl alcohol solution to transparence；Expansible graphite is weighed, is put
Enter into poly-vinyl alcohol solution, 25min is mixed with 100r/min rotating speed, powder is obtained after drying process, is then added
To boric acid aqueous solution and ferrous sulfate, stirring reaction 10min is filtered, is dried, obtain being modified expansible graphite.
Wherein, the method for preparing modified bentonite is：Bentonite is put into boric acid aqueous solution, with 100r/min's
Rotating speed mixes 30min, filters, and it is 7 to retain filter residue and be washed to pH value, after then drying filter residue under the conditions of 100 DEG C
Calcining 20min obtains the modified alta-mud.
Wherein, the water-loss reducer includes the raw material that following part is counted：1 part of cellulose ether, 1 part of polyvinyl alcohol and starch ether 0.4
Part, the preservative is sodium tetraborate, and the antifreezing agent is calcium chloride, and the waterproofing agent is waterproofing agent of organosilicon, the coloring
Agent is titanium dioxide.
Wherein, the Nano silica sol is dispersion liquid of the nanosized silica particles in water, nanometer grade silica
The mass fraction of particle is 40%, and the starch is cornstarch, and the redispersible latex powder is vinylacetate and second
Alkene copolymerization rubber powder.
A kind of preparation method of high temperature resistant environment-protective adhesive is provided in the present embodiment, comprised the following steps：
（1）, pretreatment of starch
Weigh starch to add in the water of 2 times of parts by weight, be warming up to 55 degrees Celsius, stirring obtains starch emulsion, then wherein adds
Account for the sodium hydroxide of starch quality 0.3%, then stirring reaction 10min adds and account for the potassium permanganate of starch quality 1.5% and carry out the
Then once oxidation, stirring reaction 10min adds second of the oxidation of sulfuric acid progress for accounting for starch quality 2.5%, finally to starch
Emulsion carry out suction filtration, wash to it is neutral, dehydrate and obtain pretreated starch；
（2）, prepare modified starch
Weigh sodium ethylene diamine tetracetate and step（1）Pretreated starch, be added to the water heated under 60 degrees celsius it is molten
30min is solved, 10 degrees Celsius is cooled to and obtains starch milk；
Weigh modified alta-mud to add in foregoing obtained starch milk, add sodium trimetaphosphate, it is Celsius 50 after being well mixed
20min is reacted under the conditions of degree, amido silicon oil is then added, is well mixed, modified starch slurry is obtained, then by washing, dehydration
And drying, the modified starch is obtained, it is standby；
（3）, prepare modifying epoxy resin by organosilicon
Amido silicon oil and bisphenol A epoxide resin are mixed, are dissolved in acetone, 25min, heating are stirred with 200r/min rotating speed
To 120 degrees Celsius, 50min is reacted, after reaction terminates, vacuum distillation removes acetone, obtains mixed material, diamino is added thereto
Base diphenyl-methane is mixed, and 40min is stirred with 100r/min rotating speed, dries, the silicon-modified epoxy tree is obtained after cooling
Fat, it is standby；
（4）, by step（2）Obtained modified starch and step（3）Obtained modifying epoxy resin by organosilicon mixing, is added remaining
Raw material, stirs 20min with 200r/min rotating speed, obtains the high temperature resistant environment-protective adhesive.
Embodiment 2
A kind of high temperature resistant environment-protective adhesive, includes the raw material of following part meter：70 parts of modifying epoxy resin by organosilicon, modified starch 65
Part, 35 parts of filler, 15 parts of redispersible latex powder, 25 parts of auxiliary agent and 55 parts of water；
The modifying epoxy resin by organosilicon includes the raw material that following part is counted：40 parts of bisphenol A epoxide resin, 27 parts of amido silicon oil and
18 parts of MDA；
The modified starch includes the raw material that following part is counted：16 parts of starch, amido silicon oil 12,10 parts of modified alta-mud, ethylenediamine
20 parts of 7 parts of tetraacethyl sodium, 3 parts of sodium trimetaphosphate and water；
The auxiliary agent includes the raw material that following part is counted：8 parts of water-loss reducer, 6 parts of preservative, 6 parts of antifreezing agent, 4 parts of waterproofing agent and coloring
4 parts of agent.
Wherein, the filler includes the raw material that following part is counted：It is 11 parts of wax phase change microballoon, modified 7 parts of expansible graphite, swollen
5 parts of 7 parts of swollen perlite and talcum powder.
Wherein, the wax phase change microballoon is made up of the paraffin and Opacifying polymers shell enclosed, the paraffin encapsulation
In in polymer shell.
Wherein, the Opacifying polymers shell is hollow polymer spheroid, and the hollow polymer spheroid is acrylic acid
The polymer of ester and styrene composition.
Wherein, the modified expansible graphite includes the raw material that following part is counted：2 parts of expansible graphite, 2 parts of polyvinyl alcohol,
2 parts of 1.2 parts of boric acid aqueous solution, 0.6 part of ferrous sulfate and deionized water.
Wherein, the preparation method of the modified expansible graphite is：Polyvinyl alcohol is weighed according to proportioning, deionized water is added
In, 35min is heated under the conditions of 60 DEG C, stirring and dissolving obtains poly-vinyl alcohol solution to transparence；Expansible graphite is weighed, is put
Enter into poly-vinyl alcohol solution, 30min is mixed with 150r/min rotating speed, powder is obtained after drying process, is then added
To boric acid aqueous solution and ferrous sulfate, stirring reaction 15min is filtered, is dried, obtain being modified expansible graphite.
Wherein, the method for preparing modified bentonite is：Bentonite is put into boric acid aqueous solution, with 400r/min's
Rotating speed mixes 50min, filters, and it is 7 to retain filter residue and be washed to pH value, after then drying filter residue under the conditions of 300 DEG C
Calcining 40min obtains the modified alta-mud.
Wherein, the water-loss reducer includes the raw material that following part is counted：2 parts of cellulose ether, 2 parts of polyvinyl alcohol and starch ether 0.6
Part, the preservative is sodium benzoate, and the antifreezing agent is ethylene glycol, and the waterproofing agent is nano waterproof agent, the colouring agent
For carbon black.
Wherein, the Nano silica sol is dispersion liquid of the nanosized silica particles in water, nanometer grade silica
The mass fraction of particle is 50%, and the starch is tapioca, and the redispersible latex powder is vinylacetate and second
Alkene copolymerization rubber powder.
A kind of preparation method of high temperature resistant environment-protective adhesive is provided in the present embodiment, comprised the following steps：
（1）, pretreatment of starch
Weigh starch to add in the water of 3 times of parts by weight, be warming up to 65 degrees Celsius, stirring obtains starch emulsion, then wherein adds
Account for the sodium hydroxide of starch quality 0.7%, then stirring reaction 20min adds and account for the potassium permanganate of starch quality 2.5% and carry out the
Then once oxidation, stirring reaction 15min adds second of the oxidation of sulfuric acid progress for accounting for starch quality 3%, finally to starch milk
Liquid carry out suction filtration, wash to it is neutral, dehydrate and obtain pretreated starch；
（2）, prepare modified starch
Weigh sodium ethylene diamine tetracetate and step（1）Pretreated starch, be added to the water heat at 80 degrees celsius it is molten
40min is solved, 25 degrees Celsius is cooled to and obtains starch milk；
Weigh modified alta-mud to add in foregoing obtained starch milk, add sodium trimetaphosphate, it is Celsius 70 after being well mixed
25min is reacted under the conditions of degree, amido silicon oil is then added, is well mixed, modified starch slurry is obtained, then by washing, dehydration
And drying, the modified starch is obtained, it is standby；
（3）, prepare modifying epoxy resin by organosilicon
Amido silicon oil and bisphenol A epoxide resin are mixed, are dissolved in acetone, 35min, heating are stirred with 300r/min rotating speed
To 150 degrees Celsius, 60min is reacted, after reaction terminates, vacuum distillation removes acetone, obtains mixed material, diamino is added thereto
Base diphenyl-methane is mixed, and 50min is stirred with 120r/min rotating speed, dries, the silicon-modified epoxy tree is obtained after cooling
Fat, it is standby；
（4）, by step（2）Obtained modified starch and step（3）Obtained modifying epoxy resin by organosilicon mixing, is added remaining
Raw material, stirs 30min with 300r/min rotating speed, obtains the high temperature resistant environment-protective adhesive.
Embodiment 3
A kind of high temperature resistant environment-protective adhesive, includes the raw material of following part meter：68 parts of modifying epoxy resin by organosilicon, modified starch 60
Part, 30 parts of filler, 12 parts of redispersible latex powder, 22 parts of auxiliary agent and 50 parts of water；
The modifying epoxy resin by organosilicon includes the raw material that following part is counted：35 parts of bisphenol A epoxide resin, 26 parts of amido silicon oil and
17 parts of MDA；
The modified starch includes the raw material that following part is counted：15 parts of starch, 11 parts of amido silicon oil, 9 parts of modified alta-mud, ethylenediamine
15 parts of 6 parts of tetraacethyl sodium, 2 parts of sodium trimetaphosphate and water；
The auxiliary agent includes the raw material that following part is counted：7 parts of water-loss reducer, 5 parts of preservative, 5 parts of antifreezing agent, 3 parts of waterproofing agent and coloring
3 parts of agent.
Wherein, the filler includes the raw material that following part is counted：It is 9 parts of wax phase change microballoon, modified 6 parts of expansible graphite, swollen
4 parts of 6 parts of swollen perlite and talcum powder.
Wherein, the wax phase change microballoon is made up of the paraffin and Opacifying polymers shell enclosed, the paraffin encapsulation
In in polymer shell.
Wherein, the Opacifying polymers shell is hollow polymer spheroid, and the hollow polymer spheroid is acrylic acid
The polymer of ester and styrene composition.
Wherein, the modified expansible graphite includes the raw material that following part is counted：1.5 parts of expansible graphite, polyvinyl alcohol 1.5
Part, 1 part of boric acid aqueous solution, 0.5 part of ferrous sulfate and 1.5 parts of deionized water.
Wherein, the preparation method of the modified expansible graphite is：Polyvinyl alcohol is weighed according to proportioning, deionized water is added
In, 33min is heated under the conditions of 58 DEG C, stirring and dissolving obtains poly-vinyl alcohol solution to transparence；Expansible graphite is weighed, is put
Enter into poly-vinyl alcohol solution, 27min is mixed with 125r/min rotating speed, powder is obtained after drying process, is then added
To boric acid aqueous solution and ferrous sulfate, stirring reaction 12min is filtered, is dried, obtain being modified expansible graphite.
Wherein, the method for preparing modified bentonite is：Bentonite is put into boric acid aqueous solution, with 250r/min's
Rotating speed mixes 40min, filters, and it is 7 to retain filter residue and be washed to pH value, after then drying filter residue under the conditions of 200 DEG C
Calcining 30min obtains the modified alta-mud.
Wherein, the water-loss reducer includes the raw material that following part is counted：1.5 parts of cellulose ether, 1.5 parts of polyvinyl alcohol and starch ether
0.5 part, the preservative is sodium sulfite, and the antifreezing agent is ethylene glycol, and the waterproofing agent is aluminate water-proof agent, the coloring
Agent is that titanium oxide is red.
Wherein, the Nano silica sol is dispersion liquid of the nanosized silica particles in water, nanometer grade silica
The mass fraction of particle be 45%, the starch be farina, the redispersible latex powder be vinylacetate with
Ethylene copolymer rubber powder.
A kind of preparation method of high temperature resistant environment-protective adhesive is provided in the present embodiment, comprised the following steps：
（1）, pretreatment of starch
Weigh starch to add in the water of 2.5 times of parts by weight, be warming up to 60 degrees Celsius, stirring obtains starch emulsion, then wherein add
Enter to account for the sodium hydroxide of starch quality 0.4%, then stirring reaction 15min adds and account for the potassium permanganate of starch quality 2% and carry out the
Then once oxidation, stirring reaction 12min adds second of the oxidation of sulfuric acid progress for accounting for starch quality 3%, finally to starch milk
Liquid carry out suction filtration, wash to it is neutral, dehydrate and obtain pretreated starch；
（2）, prepare modified starch
Weigh sodium ethylene diamine tetracetate and step（1）Pretreated starch, be added to the water heated under 70 degrees celsius it is molten
35min is solved, 20 degrees Celsius is cooled to and obtains starch milk；
Weigh modified alta-mud to add in foregoing obtained starch milk, add sodium trimetaphosphate, it is Celsius 60 after being well mixed
22min is reacted under the conditions of degree, amido silicon oil is then added, is well mixed, modified starch slurry is obtained, then by washing, dehydration
And drying, the modified starch is obtained, it is standby；
（3）, prepare modifying epoxy resin by organosilicon
Amido silicon oil and bisphenol A epoxide resin are mixed, are dissolved in acetone, 30min, heating are stirred with 250r/min rotating speed
To 135 degrees Celsius, 55min is reacted, after reaction terminates, vacuum distillation removes acetone, obtains mixed material, diamino is added thereto
Base diphenyl-methane is mixed, and 45min is stirred with 110r/min rotating speed, dries, the silicon-modified epoxy tree is obtained after cooling
Fat, it is standby；
（4）, by step（2）Obtained modified starch and step（3）Obtained modifying epoxy resin by organosilicon mixing, is added remaining
Raw material, stirs 25min with 250r/min rotating speed, obtains the high temperature resistant environment-protective adhesive.
The present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, its according to
The technical scheme described in foregoing embodiments can so be modified, or which part technical characteristic is equally replaced
Change.Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention
Protection domain within.
Claims (10)
1. a kind of high temperature resistant environment-protective adhesive, it is characterised in that the raw material counted including following part：Modifying epoxy resin by organosilicon 65
~ 70 parts, 55 ~ 65 parts of modified starch, 25 ~ 35 parts of filler, 10 ~ 15 parts of redispersible latex powder, 20 ~ 25 parts of auxiliary agent and water 45 ~
55 parts；
The modifying epoxy resin by organosilicon includes the raw material that following part is counted：30 ~ 40 parts of bisphenol A epoxide resin, amido silicon oil 25 ~
27 parts and 16 ~ 18 parts of MDA；
The modified starch includes the raw material that following part is counted：14 ~ 16 parts of starch, 10 ~ 12 parts of amido silicon oil, modified alta-mud 8 ~ 10
10 ~ 20 parts of part, 5 ~ 7 parts of sodium ethylene diamine tetracetate, 1 ~ 3 part of sodium trimetaphosphate and water；
The auxiliary agent includes the raw material that following part is counted：6 ~ 8 parts of water-loss reducer, 4 ~ 6 parts of preservative, 4 ~ 6 parts of antifreezing agent, waterproofing agent 2 ~ 4
2 ~ 4 parts of part and colouring agent.
2. high temperature resistant environment-protective adhesive according to claim 1, it is characterised in that the filler includes the original that following part is counted
Material：3 ~ 5 parts of 8 ~ 11 parts of wax phase change microballoon, modified 5 ~ 7 parts of expansible graphite, 5 ~ 7 parts of expanded perlite and talcum powder.
3. high temperature resistant environment-protective adhesive according to claim 2, it is characterised in that the wax phase change microballoon is by enclosing
Paraffin and Opacifying polymers shell composition, the paraffin are packaged in polymer shell.
4. high temperature resistant environment-protective adhesive according to claim 3, it is characterised in that the Opacifying polymers shell is sky
Heart polymer spheres, the hollow polymer spheroid is the polymer that acrylate and styrene are constituted.
5. high temperature resistant environment-protective adhesive according to claim 2, it is characterised in that the modified expansible graphite include with
The raw material of lower part meter：1 ~ 2 part of expansible graphite, 1 ~ 2 part of polyvinyl alcohol, 0.8 ~ 1.2 part of boric acid aqueous solution, ferrous sulfate 0.4 ~
0.6 part and 1 ~ 2 part of deionized water.
6. high temperature resistant environment-protective adhesive according to claim 5, it is characterised in that the preparation of the modified expansible graphite
Method is：Polyvinyl alcohol is weighed according to proportioning, is added in deionized water, 30 ~ 35min is heated under the conditions of 55 ~ 60 DEG C, is stirred molten
Solution obtains poly-vinyl alcohol solution to transparence；Expansible graphite is weighed, is put into poly-vinyl alcohol solution, with 100 ~ 150r/
Min rotating speed mixes 25 ~ 30min, and powder is obtained after drying process, is then added to boric acid aqueous solution and ferrous sulfate,
10 ~ 15min of stirring reaction, is filtered, and is dried, is obtained being modified expansible graphite.
7. high temperature resistant environment-protective adhesive according to claim 1, it is characterised in that the method for preparing modified bentonite
For：Bentonite is put into boric acid aqueous solution, 30 ~ 50min is mixed with 100 ~ 400r/min rotating speed, filtering retains filter
Slag is simultaneously washed to pH value for 7, and 20 ~ 40min is calcined under the conditions of 100 ~ 300 DEG C after then filter residue is dried, and to obtain the modification swollen
Profit soil.
8. high temperature resistant environment-protective adhesive according to claim 1, it is characterised in that the water-loss reducer includes what following part was counted
Raw material：0.4 ~ 0.6 part of 1 ~ 2 part of cellulose ether, 1 ~ 2 part of polyvinyl alcohol and starch ether, the preservative are sodium tetraborate, benzoic acid
One or more in sodium, natrium nitrosum, sodium sulfite and triethanolamine, the antifreezing agent be calcium chloride or ethylene glycol, it is described
Waterproofing agent be waterproofing agent of organosilicon, nano waterproof agent and aluminate water-proof agent in one or more, the colouring agent be titanium dioxide,
Carbon black, titanium oxide are red, any of iron oxide yellow and barba hispanica.
9. high temperature resistant environment-protective adhesive according to claim 1, it is characterised in that the Nano silica sol is nanoscale two
Dispersion liquid of the silicon oxide particle in water, the mass fraction of nanosized silica particles is 40 ~ 50%, and the starch is corn
Starch, tapioca, the one or more of farina and wheaten starch, the redispersible latex powder are vinyl acetate
Ester and ethylene copolymer rubber powder.
10. a kind of preparation method of high temperature resistant environment-protective adhesive according to any one of claim 1 ~ 9, it is characterised in that
Comprise the following steps：
（1）, pretreatment of starch
Weigh starch to add in the water of 2 ~ 3 times of parts by weight, be warming up to 55 ~ 65 degrees Celsius, stirring obtains starch emulsion, then wherein
Addition accounts for the sodium hydroxide of starch quality 0.3 ~ 0.7%, and then 10 ~ 20min of stirring reaction adds and account for starch quality 1.5 ~ 2.5%
Potassium permanganate carry out first time oxidation, 10 ~ 15min of stirring reaction, then add account for starch quality 2.5 ~ 3% sulfuric acid carry out
Second aoxidizes, finally starch emulsion is carried out suction filtration, wash to it is neutral, dehydrate and obtain pretreated starch；
（2）, prepare modified starch
Weigh sodium ethylene diamine tetracetate and step（1）Pretreated starch, is added to the water and is heated under 60 ~ 80 degrees celsius
30 ~ 40min is dissolved, 10 ~ 25 degrees Celsius is cooled to and obtains starch milk；
Weigh modified alta-mud to add in foregoing obtained starch milk, add sodium trimetaphosphate, taken the photograph after being well mixed 50 ~ 70
20 ~ 25min is reacted under the conditions of family name's degree, amido silicon oil is then added, is well mixed, obtains modified starch slurry, then by washing,
It is dehydrated and dries, obtains the modified starch, it is standby；
（3）, prepare modifying epoxy resin by organosilicon
Amido silicon oil and bisphenol A epoxide resin are mixed, are dissolved in acetone, with 200 ~ 300r/min rotating speed stirring 25 ~
35min, is warming up to 120 ~ 150 degrees Celsius, reacts 50 ~ 60min, and after reaction terminates, vacuum distillation removes acetone, obtains mixture
Material, adds MDA mixing, 40 ~ 50min is stirred with 100 ~ 120r/min rotating speed, dry, after cooling thereto
The modifying epoxy resin by organosilicon is obtained, it is standby；
（4）, by step（2）Obtained modified starch and step（3）Obtained modifying epoxy resin by organosilicon mixing, is added remaining
Raw material, stirs 20 ~ 30min with 200 ~ 300r/min rotating speed, obtains the high temperature resistant environment-protective adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710644697.XA CN107286889A (en) | 2017-08-01 | 2017-08-01 | A kind of high temperature resistant environment-protective adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710644697.XA CN107286889A (en) | 2017-08-01 | 2017-08-01 | A kind of high temperature resistant environment-protective adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107286889A true CN107286889A (en) | 2017-10-24 |
Family
ID=60104632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710644697.XA Withdrawn CN107286889A (en) | 2017-08-01 | 2017-08-01 | A kind of high temperature resistant environment-protective adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107286889A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047988A (en) * | 2017-11-25 | 2018-05-18 | 宁波斯凯勒智能科技有限公司 | It is a kind of for adhesive of furniture and preparation method thereof |
| CN109021877A (en) * | 2018-07-04 | 2018-12-18 | 合肥尚涵装饰工程有限公司 | A kind of wallpaper adhesive of water proof and wearable |
| CN114507500A (en) * | 2022-04-08 | 2022-05-17 | 山东格润高分子材料有限公司 | Cooking-resistant modified polyurethane adhesive and preparation method thereof |
| CN114561180A (en) * | 2022-04-08 | 2022-05-31 | 山东格润高分子材料有限公司 | High-temperature-resistant environment-friendly adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571374A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Fireproof hot melt adhesive for automotive upholstery |
| CN106479413A (en) * | 2015-08-28 | 2017-03-08 | 开县庆宁木业有限公司 | The formaldehydeless bonding agent of sheet material |
| CN106479416A (en) * | 2015-08-28 | 2017-03-08 | 开县庆宁木业有限公司 | Multifunction adhesive |
-
2017
- 2017-08-01 CN CN201710644697.XA patent/CN107286889A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571374A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Fireproof hot melt adhesive for automotive upholstery |
| CN106479413A (en) * | 2015-08-28 | 2017-03-08 | 开县庆宁木业有限公司 | The formaldehydeless bonding agent of sheet material |
| CN106479416A (en) * | 2015-08-28 | 2017-03-08 | 开县庆宁木业有限公司 | Multifunction adhesive |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047988A (en) * | 2017-11-25 | 2018-05-18 | 宁波斯凯勒智能科技有限公司 | It is a kind of for adhesive of furniture and preparation method thereof |
| CN109021877A (en) * | 2018-07-04 | 2018-12-18 | 合肥尚涵装饰工程有限公司 | A kind of wallpaper adhesive of water proof and wearable |
| CN114507500A (en) * | 2022-04-08 | 2022-05-17 | 山东格润高分子材料有限公司 | Cooking-resistant modified polyurethane adhesive and preparation method thereof |
| CN114561180A (en) * | 2022-04-08 | 2022-05-31 | 山东格润高分子材料有限公司 | High-temperature-resistant environment-friendly adhesive and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107286889A (en) | A kind of high temperature resistant environment-protective adhesive and preparation method thereof | |
| CN104031417B (en) | A kind of modified calcium carbonate with heat insulation and preservation effect and preparation method thereof | |
| CN107201159A (en) | A kind of cracking resistance, anti-dropout coating and preparation method | |
| CN104087027B (en) | A kind of heat resist modification calcium carbonate and preparation method thereof | |
| CN103254888A (en) | Clean-water carrying fracturing supporting agent and preparation method | |
| CN104084175B (en) | A kind of modified calcium carbonate with adsorption effect and preparation method thereof | |
| CN107177334B (en) | A kind of gap filler and preparation method thereof with antibacterial functions | |
| CN107236507A (en) | It is a kind of for the high-temperature resistance adhesive on floor and preparation method thereof | |
| CN105418775A (en) | Cross-linked carboxymethyl hydroxypropylated compound modified starch and preparation method thereof | |
| CN108505392A (en) | The preparation method of nanomete talc powder | |
| CN104452424A (en) | Waterproof and heat-resistant stiff PVC wallpaper base paper and preparation method thereof | |
| CN105155292A (en) | Production method of environmentally friendly leather imitation synthetic leather | |
| CN109486441A (en) | A kind of corrugated board low temperature adhesion glue | |
| CN108624257A (en) | A kind of modified meerschaum EVA hot-melt adhesive | |
| CN108405797A (en) | A kind of preparation method of the water base cast paint of quick-drying higher suspension | |
| CN104774522A (en) | Heat insulation paint preparation method | |
| CN108441141A (en) | A kind of compound polyvinyl acetate emulsion adhesive | |
| CN106995637A (en) | A kind of water proof anti-seepage material and preparation method thereof | |
| CN104909626A (en) | Fire retardant insulation mortar for building's exterior and preparation method thereof | |
| CN107502227B (en) | A kind of non-ionic starch based adhesive and preparation method thereof | |
| CN109401435A (en) | A kind of abrasion-resistance water ink and its preparation process | |
| CN104774508B (en) | Preparation method of modified heat-insulating coating | |
| CN107141515A (en) | Decorative joint mixture and preparation method thereof | |
| CN106566308A (en) | Cross-linked polyethyleneimine-modified calcium carbonate powder for waterborne paint and preparation method thereof | |
| CN106590045A (en) | Polymethyl methacrylate-nano cerium oxide coating modification calcium carbonate powder and preparing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20171024 |