CN108624285A - A kind of preparation method of water-resistant type soy protein adhesives - Google Patents
A kind of preparation method of water-resistant type soy protein adhesives Download PDFInfo
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- CN108624285A CN108624285A CN201810537700.2A CN201810537700A CN108624285A CN 108624285 A CN108624285 A CN 108624285A CN 201810537700 A CN201810537700 A CN 201810537700A CN 108624285 A CN108624285 A CN 108624285A
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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
- C09J189/00—Adhesives based on proteins; Adhesives based on derivatives thereof
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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Abstract
The invention discloses a kind of preparation methods of water-resistant type soy protein adhesives, belong to chemical adhesive technical field.After soybean protein and water are first stirred by the present invention, endopeptidase, constant temperature stirring enzymolysis, then heated heating enzyme deactivation are added, it is cooling, obtain enzymolysis liquid；Enzymolysis liquid is added in reaction kettle again, pH to 3.2~3.4 is adjusted, adds linoleic acid, linseed oil and carbodiimides, constant temperature is stirred to react, and is concentrated under reduced pressure, is obtained concentrate；Then concentrate, cosolvent, melamine, molysite, filler and preservative heating stirring are mixed, then adjust pH, is continued after being stirred, is discharged to get water-resistant type soy protein adhesives.Water-resistant type soy protein adhesives prepared by technical solution of the present invention have the characteristics that excellent water resistance energy and adhesion strength, have broad prospects in the development of chemical adhesive technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of water-resistant type soy protein adhesives, belong to chemical adhesive technology neck
Domain.
Background technology
Soybean protein base adhesive is a kind of Environment-friendlyadhesive adhesive, has abundant raw material, reactivity high and easy to operate
And cementitious product the features such as being discharged without free formaldehyde, it is increasingly subject to the attention and favor of people.But bonding strength is low and water-fast
Performance it is poor be always limitation soybean protein base adhesive development bottleneck problem, thus people take different methods to its into
Row is modified.Research confirmation, the crosslinking of degrees of functionality >=2 such as glyoxal, glutaraldehyde, dicyandiamide, maleic anhydride, polyisocyanates
Agent can be reacted with soybean protein residue.Such crosslinking agent is by the cross-linking reaction with residue, time to soybean protein destructible
Level structure is supplemented and is enhanced, final to improve the resistance to of soy protein adhesives to increase the cohesive strength of adhesive itself
Aqueous and bonding strength.Having researcher's early period, to be prepared for water resistance preferable by cross-linking modified on the basis of alkaline degradation is modified
Soy protein adhesives.In research, the effect of alkali essentially consists in the hydrogen bond destroyed between protein molecule, reduces the glutinous of adhesive
Degree.In practical R＆D process, in order to reach the viscosity with operability, the alkali number used is usually higher, reaches solid bean powder
The 8% of amount is even higher.But constantly degraded because of the long-term existence of alkali using the bean gum that alkaline degradation is modified, so that system is become not
Stablize, seriously affects the storage stability of bean gum.Stabilizer is added in the legumin liquid of degradation, the functional group in bean gum obtains
To improvement, storage stability improves, moreover it is possible to which activation is reacted with the further of follow-up crosslinking agent.The soybean protein of degradation, exposure
Go out the groups such as-NH2 ,-CONH ,-SH, there may be extremely strong affinity with-CH2OH, be the steady of soybean protein degradation solution
Surely theoretical foundation is provided.But traditional soybean protein base adhesive there is also water resistances and adhesive strength can not be further
It improves.
Therefore, how to improve traditional soybean albumen base adhesive there is also water resistances and adhesive strength further to carry
High disadvantage is the problem of it need to be researched and solved to obtain more high combination property.
Invention content
The present invention solves the technical problem of：For traditional soybean protein base adhesive there is also water resistance and
The shortcomings that adhesive strength can not further increase provides a kind of preparation method of water-resistant type soy protein adhesives.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of water-resistant type soy protein adhesives, specific preparation process are；
（1）It counts in parts by weight, takes 20~30 portions of soybean proteins, 2~4 parts of endopeptidases, 180~200 parts of water, first by soybean successively
After albumen and water are stirred, endopeptidase, constant temperature stirring enzymolysis, then heated heating enzyme deactivation are added, it is cooling, obtain enzymolysis liquid；
（2）It counts in parts by weight, takes 8~10 parts of linoleic acid successively, 30~40 portions of linseed oil, 2~4 parts of carbodiimides, 100~
First enzymolysis liquid is added in reaction kettle for 150 parts of enzymolysis liquids, adjusts pH to 3.2~3.4, adds linoleic acid, linseed oil and carbonization
Diimine, constant temperature are stirred to react, and are concentrated under reduced pressure, are obtained concentrate；
（3）It counts in parts by weight, takes 80~100 portions of concentrates successively, 8~10 parts of cosolvents, 3~5 parts of melamines, 0.1~
0.2 part of molysite, 10~15 parts of fillers, 1~3 portion of preservative, heating stirring mixing, then pH to 4.5~5.0 is adjusted, continue to stir
Mixing discharges to get water-resistant type soy protein adhesives.
Step（1）The endopeptidase is any one in trypsase, chymotrypsin or elastoser.
Step（3）It is 10 in mass ratio that the cosolvent, which is by glycerine and ethylene glycol,：1~15：1 compounds.
Step（3）The molysite is any one in iron chloride, ferric nitrate or ferric sulfate.
Step（3）The filler is any one in gas-phase silica or graphene oxide.
Step（3）The preservative is potassium sorbate, sodium benzoate, in dehydroactic acid sodium or butyl p-hydroxybenzoate
Any one.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is first hydrolyzed soybean protein using endopeptidase, under endopeptidase effect, protein hair
Raw initial hydrolysis, the polypeptide of small molecule is hydrolyzed to from the protein of macromolecular, living to make the tertiary structure of soybean protein disintegrate
Property number of functional groups increase, reactivity is improved, then using linoleic acid as modifying agent, pass through carbodiimides mediate it is anti-
It answers, linoleic acid is coupled on peptide molecule chain, first, containing unsaturated carbon-carbon double bond in linoleic acid molecular structure, therefore can
The antioxygenic property of product is improved, secondly, long alkane chain is exposed on the outside of peptide molecule structure in linoleic acid molecular structure, is improved
Water resistance on the outside of peptide molecule, meanwhile, the generation of the structure is conducive to improve linseed oil and the interface of polypeptide is described
Property, so that linseed oil is penetrated into inside polypeptide colloform texture, to make flax oil component occupy polypeptide colloform texture interior section
The position of functional group makes the free radical amount that can form hydrophilic bond inside colloid with water reduce, makes water resistance inside colloid
Synchronous lifting is obtained, in addition, linseed oil is drying oil, during product adhesive solidification, linseed oil is cured, to be formed
The linseed oil film of hydrophobic structure, the water resistance after making product cure further are promoted；
（2）Technical solution of the present invention is carried in melamine molecule structure by adding melamine and molysite first first
Primary amino group and secondary amino group can be with the oxygen-containing functional groups in inorganic filler（Hydroxyl, carboxyl etc.）Hydrogen bond is formed, it is inorganic to be conducive to
Distribution of the filler in adhesive system, and melamine can be used as crosslinking agent, the protein after making enzymolysis activate occurs again
Crosslinking, forms new cross-linked network structure, to improve the adhesive strength of adhesive product, furthermore, by adding molysite, molysite
The iron ion ionized out can be chelated with protein, to make protein interior form physical crosslinking, make cross-linked network density
It is further promoted, bond properties is further promoted, and the chelating of iron ion and protein, can be made hydrophilic in protein molecule
Group transfer avoids the problem that hydrophilic radical occur after product cures causes water resistance to decline on the outside to inside.
Specific implementation mode
It counts in parts by weight, takes 20~30 portions of soybean proteins successively, 2~4 parts of endopeptidases, 180~200 parts of water first will be big
Legumin and water mixing are poured into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, are in temperature
35~36 DEG C, under the conditions of rotating speed is 400~800r/min, after constant temperature is stirred 20~30min, endopeptidase is added, is continued
After constant temperature stirs 2~4h of enzyme digestion reaction, 90~95 DEG C are heated to, after keeping the temperature 10~20min of enzyme deactivation, naturally cools to room
Temperature, discharging, obtains enzymolysis liquid；It counts in parts by weight, takes 8~10 parts of linoleic acid, 30~40 portions of linseed oil, 2~4 parts of carbonizations two successively
First enzymolysis liquid is added in reaction kettle for imines, 100~150 parts of enzymolysis liquids, adjusts enzymolysis liquid pH to 3.2~3.4 in reaction kettle,
Wait for pH adjust after, add linoleic acid, linseed oil and carbodiimides, then in temperature be 65~70 DEG C, rotating speed 600
Under the conditions of~800r/min, after constant temperature is stirred to react 4~6h, material in reaction kettle is transferred in Rotary Evaporators, is in temperature
75~85 DEG C, under the conditions of pressure is 500~520kPa, 30~40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, successively
Take 80~100 portions of concentrates, 8~10 parts of cosolvents, 3~5 parts of melamines, 0.1~0.2 part of molysite, 10~15 parts of fillers, 1
~3 portions of preservatives, be added batch mixer in, in rotating speed be 800~1200r/min, temperature be 58~65 DEG C under the conditions of, heating stirring
After mixing 2~3h, material pH to 4.5~5.0 in batch mixer is adjusted, after waiting for that pH is adjusted, continue to be stirred 20~
30min discharges to get water-resistant type soy protein adhesives.The endopeptidase is trypsase, chymotrypsin or elastoser
In any one.It is 10 in mass ratio that the cosolvent, which is by glycerine and ethylene glycol,：1~15：1 compounds.The molysite
For any one in iron chloride, ferric nitrate or ferric sulfate.The filler is arbitrary in gas-phase silica or graphene oxide
It is a kind of.The preservative is potassium sorbate, sodium benzoate, any one in dehydroactic acid sodium or butyl p-hydroxybenzoate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts reaction
Enzymolysis liquid pH to 3.4 in kettle adds linoleic acid, linseed oil and carbodiimides, is in temperature then after waiting for that pH is adjusted
70 DEG C, under the conditions of rotating speed is 800r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, in
Temperature is 85 DEG C, under the conditions of pressure is 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 parts successively
Concentrate, 10 parts of cosolvents, 5 parts of melamines, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in turn
Speed is 1200r/min, under the conditions of temperature is 65 DEG C, after heating stirring mixes 3h, adjusts material pH to 5.0 in batch mixer, waits for pH
After adjusting, continues to be stirred 30min, discharge to get water-resistant type soy protein adhesives.The endopeptidase is tryptose
Enzyme.It is 15 in mass ratio that the cosolvent, which is by glycerine and ethylene glycol,：1 compounds.The molysite is iron chloride.The filler
For gas-phase silica.The preservative is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of peptide ending enzymes, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, peptide ending enzyme is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts reaction
Enzymolysis liquid pH to 3.4 in kettle adds linoleic acid, linseed oil and carbodiimides, is in temperature then after waiting for that pH is adjusted
70 DEG C, under the conditions of rotating speed is 800r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, in
Temperature is 85 DEG C, under the conditions of pressure is 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 parts successively
Concentrate, 10 parts of cosolvents, 5 parts of melamines, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in turn
Speed is 1200r/min, under the conditions of temperature is 65 DEG C, after heating stirring mixes 3h, adjusts material pH to 5.0 in batch mixer, waits for pH
After adjusting, continues to be stirred 30min, discharge to get water-resistant type soy protein adhesives.The cosolvent is by glycerine
It is 15 in mass ratio with ethylene glycol：1 compounds.The molysite is iron chloride.The filler is gas-phase silica.The anti-corrosion
Agent is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 40 successively
First enzymolysis liquid is added in reaction kettle for part linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts enzymolysis liquid in reaction kettle
PH to 3.4, wait for pH adjust after, add linseed oil and carbodiimides, then in temperature be 70 DEG C, rotating speed 800r/
Under the conditions of min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, is 85 DEG C in temperature, pressure is
Under the conditions of 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 portions of concentrates, 10 parts of hydrotropies successively
Agent, 5 parts of melamines, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in rotating speed be 1200r/min, temperature
Under the conditions of degree is 65 DEG C, after heating stirring mixes 3h, material pH to 5.0 in batch mixer is adjusted, after waiting for that pH is adjusted, continues to stir
Mixing 30min is mixed, is discharged to get water-resistant type soy protein adhesives.The endopeptidase is trypsase.The cosolvent be by
Glycerine and ethylene glycol are 15 in mass ratio：1 compounds.The molysite is iron chloride.The filler is gas-phase silica.It is described
Preservative is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts enzymolysis liquid in reaction kettle
PH to 3.4, wait for pH adjust after, add linoleic acid and carbodiimides, then in temperature be 70 DEG C, rotating speed 800r/
Under the conditions of min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, is 85 DEG C in temperature, pressure is
Under the conditions of 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 portions of concentrates, 10 parts of hydrotropies successively
Agent, 5 parts of melamines, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in rotating speed be 1200r/min, temperature
Under the conditions of degree is 65 DEG C, after heating stirring mixes 3h, material pH to 5.0 in batch mixer is adjusted, after waiting for that pH is adjusted, continues to stir
Mixing 30min is mixed, is discharged to get water-resistant type soy protein adhesives.The endopeptidase is trypsase.The cosolvent be by
Glycerine and ethylene glycol are 15 in mass ratio：1 compounds.The molysite is iron chloride.The filler is gas-phase silica.It is described
Preservative is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 40 portions of linseed oil, 150 parts of enzymolysis liquids, adjust in reaction kettle enzymolysis liquid pH to
3.4, wait for pH adjust after, add linoleic acid, linseed oil, then in temperature be 70 DEG C, rotating speed be 800r/min under the conditions of,
After constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, is 85 DEG C in temperature, pressure is 520kPa conditions
Under, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 portions of concentrates, 10 parts of cosolvents, 5 parts of melamines successively
Amine, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives are added in batch mixer, are 1200r/min in rotating speed, temperature is 65 DEG C of conditions
Under, after heating stirring mixes 3h, material pH to 5.0 in batch mixer is adjusted, after waiting for that pH is adjusted, continues to be stirred 30min,
Discharging is to get water-resistant type soy protein adhesives.The endopeptidase is trypsase.The cosolvent is by glycerine and ethylene glycol
It is 15 in mass ratio：1 compounds.The molysite is iron chloride.The filler is gas-phase silica.The preservative is sorb
Sour potassium.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts reaction
Enzymolysis liquid pH to 3.4 in kettle adds linoleic acid, linseed oil and carbodiimides, is in temperature then after waiting for that pH is adjusted
70 DEG C, under the conditions of rotating speed is 800r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, in
Temperature is 85 DEG C, under the conditions of pressure is 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 parts successively
Concentrate, 10 parts of cosolvents, 0.2 part of molysite, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in rotating speed be 1200r/
Min under the conditions of temperature is 65 DEG C, after heating stirring mixes 3h, adjusts material pH to 5.0 in batch mixer, after waiting for that pH is adjusted,
Continue to be stirred 30min, discharge to get water-resistant type soy protein adhesives.The endopeptidase is trypsase.The hydrotropy
It is 15 in mass ratio that agent, which is by glycerine and ethylene glycol,：1 compounds.The molysite is iron chloride.The filler is gas phase hard charcoal
It is black.The preservative is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
First enzymolysis liquid is added in reaction kettle for part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids, adjusts reaction
Enzymolysis liquid pH to 3.4 in kettle adds linoleic acid, linseed oil and carbodiimides, is in temperature then after waiting for that pH is adjusted
70 DEG C, under the conditions of rotating speed is 800r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, in
Temperature is 85 DEG C, under the conditions of pressure is 520kPa, 40min is concentrated under reduced pressure, obtains concentrate；It counts in parts by weight, takes 100 parts successively
Concentrate, 10 parts of cosolvents, 5 parts of melamines, 15 parts of fillers, 3 portions of preservatives, be added batch mixer in, in rotating speed be 1200r/
Min under the conditions of temperature is 65 DEG C, after heating stirring mixes 3h, adjusts material pH to 5.0 in batch mixer, after waiting for that pH is adjusted,
Continue to be stirred 30min, discharge to get water-resistant type soy protein adhesives.The endopeptidase is trypsase.The hydrotropy
It is 15 in mass ratio that agent, which is by glycerine and ethylene glycol,：1 compounds.The filler is gas-phase silica.The preservative is mountain
Potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
Enzymolysis liquid is first added in reaction kettle, adds Asia by part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids
Oleic acid, linseed oil and carbodiimides are then 70 DEG C in temperature, and under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 6h
Afterwards, material in reaction kettle is transferred in Rotary Evaporators, is 85 DEG C in temperature, under the conditions of pressure is 520kPa, is concentrated under reduced pressure
40min obtains concentrate；It counts in parts by weight, takes 100 portions of concentrates, 10 parts of cosolvents, 5 parts of melamines, 0.2 part of iron successively
Salt, 15 parts of fillers, 3 portions of preservatives are added in batch mixer, are 1200r/min in rotating speed, under the conditions of temperature is 65 DEG C, heating is stirred
After mixing mixing 3h, adjust material pH to 5.0 in batch mixer, after waiting for that pH is adjusted, continue to be stirred 30min, discharging to get
Water-resistant type soy protein adhesives.The endopeptidase is trypsase.The cosolvent be by glycerine and ethylene glycol in mass ratio
It is 15：1 compounds.The molysite is iron chloride.The filler is gas-phase silica.The preservative is potassium sorbate.
It counts in parts by weight, 30 portions of soybean proteins, 4 parts of endopeptidases, 200 parts of water is taken first to mix soybean protein and water successively
It pours into No. 1 beaker, and No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, be 36 DEG C in temperature, rotating speed is
Under the conditions of 800r/min, after constant temperature is stirred 30min, endopeptidase is added, after continuing constant temperature stirring enzyme digestion reaction 4h, heating
95 DEG C are warming up to, after keeping the temperature enzyme deactivation 20min, cooled to room temperature, discharging obtains enzymolysis liquid；It counts in parts by weight, takes 10 successively
Enzymolysis liquid is first added in reaction kettle, adds Asia by part linoleic acid, 40 portions of linseed oil, 4 parts of carbodiimides, 150 parts of enzymolysis liquids
Oleic acid, linseed oil and carbodiimides are then 70 DEG C in temperature, and under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 6h
Afterwards, material in reaction kettle is transferred in Rotary Evaporators, is 85 DEG C in temperature, under the conditions of pressure is 520kPa, is concentrated under reduced pressure
40min obtains concentrate；It counts in parts by weight, takes 100 portions of concentrates, 10 parts of cosolvents, 5 parts of melamines, 0.2 part of iron successively
Salt, 15 parts of fillers, 3 portions of preservatives are added in batch mixer, are 1200r/min in rotating speed, under the conditions of temperature is 65 DEG C, heating is stirred
After mixing mixing 3h, continues to be stirred 30min, discharge to get water-resistant type soy protein adhesives.The endopeptidase is tryptose
Enzyme.It is 15 in mass ratio that the cosolvent, which is by glycerine and ethylene glycol,：1 compounds.The molysite is iron chloride.The filler
For gas-phase silica.The preservative is potassium sorbate.
Comparative example：The soy protein adhesives of Guangdong Science and Technology Ltd. production.
The water-resistant type soy protein adhesives and comparative example product of example 1 to 9 gained of example are subjected to performance detection, specifically
Detection method is as follows：
Experiment plank is particieboard, and dimensions is 250mm × 250mm × 10mm, is glued in a manner of glue spraying, resin added 10%（Glue
Solid content accounts for over dry wood shavings）.Using three-stage hot-pressing process curve, hot pressing pressure 1.6MPa, hot pressing temperature is 180 DEG C, heat
The pressure time is 9min.The plank prepared measures bonding strength in its dry shape, the expansion of 2h water sucting thickness after sanding surface is handled
Rate.Measurement method is referring to GB/T17657.
Specific testing result is as shown in table 1：
1 water-resistant type soy protein adhesives performance test results of table
By 1 testing result of table it is found that water-resistant type soy protein adhesives prepared by technical solution of the present invention have excellent water resistance
It the characteristics of energy and adhesion strength, has broad prospects in the development of chemical adhesive technology industry.
Claims (6)
1. a kind of preparation method of water-resistant type soy protein adhesives, which is characterized in that specifically preparation process is；
（1）It counts in parts by weight, takes 20~30 portions of soybean proteins, 2~4 parts of endopeptidases, 180~200 parts of water, first by soybean successively
After albumen and water are stirred, endopeptidase, constant temperature stirring enzymolysis, then heated heating enzyme deactivation are added, it is cooling, obtain enzymolysis liquid；
（2）It counts in parts by weight, takes 8~10 parts of linoleic acid successively, 30~40 portions of linseed oil, 2~4 parts of carbodiimides, 100~
First enzymolysis liquid is added in reaction kettle for 150 parts of enzymolysis liquids, adjusts pH to 3.2~3.4, adds linoleic acid, linseed oil and carbonization
Diimine, constant temperature are stirred to react, and are concentrated under reduced pressure, are obtained concentrate；
（3）It counts in parts by weight, takes 80~100 portions of concentrates successively, 8~10 parts of cosolvents, 3~5 parts of melamines, 0.1~
0.2 part of molysite, 10~15 parts of fillers, 1~3 portion of preservative, heating stirring mixing, then pH to 4.5~5.0 is adjusted, continue to stir
Mixing discharges to get water-resistant type soy protein adhesives.
2. a kind of preparation method of water-resistant type soy protein adhesives according to claim 1, which is characterized in that step
（1）The endopeptidase is any one in trypsase, chymotrypsin or elastoser.
3. a kind of preparation method of water-resistant type soy protein adhesives according to claim 1, which is characterized in that step
（3）It is 10 in mass ratio that the cosolvent, which is by glycerine and ethylene glycol,：1~15：1 compounds.
4. a kind of preparation method of water-resistant type soy protein adhesives according to claim 1, which is characterized in that step
（3）The molysite is any one in iron chloride, ferric nitrate or ferric sulfate.
5. a kind of preparation method of water-resistant type soy protein adhesives according to claim 1, which is characterized in that step
（3）The filler is any one in gas-phase silica or graphene oxide.
6. a kind of preparation method of water-resistant type soy protein adhesives according to claim 1, which is characterized in that step
（3）The preservative is potassium sorbate, sodium benzoate, any one in dehydroactic acid sodium or butyl p-hydroxybenzoate.
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| CN109517577A (en) * | 2018-11-23 | 2019-03-26 | 北京林业大学 | A kind of toughness dregs of beans albumen adhesive and preparation method thereof |
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| CN109504343B (en) * | 2018-11-23 | 2022-01-28 | 北京林业大学 | Formaldehyde-free bean gum and preparation method thereof |
| CN109517577B (en) * | 2018-11-23 | 2022-01-28 | 北京林业大学 | Tough soybean meal protein adhesive and preparation method thereof |
| CN109517576B (en) * | 2018-11-23 | 2022-01-28 | 北京林业大学 | Aldehyde-free protein adhesive and preparation method thereof |
| CN109554160B (en) * | 2018-11-23 | 2022-02-11 | 北京林业大学 | Aldehyde-free soybean meal protein adhesive and preparation method thereof |
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