CN108624285B - Preparation method of water-resistant soybean protein adhesive - Google Patents
Preparation method of water-resistant soybean protein adhesive Download PDFInfo
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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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- 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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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a preparation method of a water-resistant soybean protein adhesive, belonging to the technical field of chemical adhesives. Stirring and mixing soybean protein and water, adding endopeptidase, stirring and carrying out enzymolysis at constant temperature, heating to inactivate enzyme, and cooling to obtain an enzymolysis solution; adding the enzymatic hydrolysate into a reaction kettle, adjusting the pH to 3.2-3.4, adding linoleic acid, linseed oil and carbodiimide, stirring at constant temperature for reaction, and concentrating under reduced pressure to obtain a concentrated solution; and then heating, stirring and mixing the concentrated solution, the cosolvent, melamine, ferric salt, the filler and the preservative, adjusting the pH value, continuously stirring and mixing, and discharging to obtain the water-resistant soy protein adhesive. The water-resistant soy protein adhesive prepared by the technical scheme of the invention has the characteristics of excellent water resistance and bonding strength, and has wide prospects in the development of the chemical adhesive technology industry.
Description
Technical Field
The invention discloses a preparation method of a water-resistant soybean protein adhesive, belonging to the technical field of chemical adhesives.
Background
The soybean protein-based adhesive is an environment-friendly adhesive, has the characteristics of rich raw materials, high reaction activity, simplicity in operation, no free formaldehyde release of a bonded product and the like, and is increasingly valued and favored by people. However, the low bonding strength and poor water resistance have been bottleneck problems limiting the development of soy protein based adhesives, and thus, different methods have been adopted to modify them. It has been confirmed that cross-linking agents having a functionality of 2 or more, such as glyoxal, glutaraldehyde, dicyandiamide, maleic anhydride, polyisocyanate, etc., can react with the soybean protein residue. The crosslinking agent supplements and strengthens a secondary structure which is easy to damage the soybean protein through a crosslinking reaction with residues, so that the cohesive strength of the adhesive is increased, and the water resistance and the bonding strength of the soybean protein adhesive are finally improved. Researchers prepare the soybean protein adhesive with better water resistance through crosslinking modification on the basis of alkali degradation modification in the early stage. In research, the alkali mainly acts on breaking hydrogen bonds among protein molecules and reducing the viscosity of the adhesive. In actual development, the amount of alkali used is generally high, up to 8% or more of the amount of solid soy flour, in order to achieve a workable viscosity. However, the soybean gums modified by alkali degradation are degraded continuously due to the long-term presence of alkali, so that the system becomes unstable, and the storage stability of the soybean gums is seriously affected. The stabilizer is added into the degraded soybean protein liquid, so that the functional group in the soybean gum is improved, the storage stability is improved, and the further reaction with a subsequent cross-linking agent can be activated. The degraded soybean protein exposes-NH 2, -CONH, -SH and other groups, and may have strong affinity with-CH 2OH, thereby providing a theoretical basis for the stability of the soybean protein degradation solution. However, the water resistance and the adhesive strength of the conventional soy protein-based adhesives cannot be further improved.
Therefore, how to improve the defects that the water resistance and the bonding strength of the traditional soy protein-based adhesive cannot be further improved so as to obtain higher comprehensive performance is a problem to be researched and solved.
Disclosure of Invention
The invention mainly solves the technical problems that: aiming at the defect that the water resistance and the bonding strength of the traditional soy protein-based adhesive cannot be further improved, the preparation method of the water-resistant soy protein adhesive is provided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a water-resistant soy protein adhesive comprises the following specific steps of;
(1) taking 20-30 parts of soybean protein, 2-4 parts of endopeptidase and 180-200 parts of water in sequence by weight, firstly stirring and mixing the soybean protein and the water, then adding the endopeptidase, stirring and carrying out enzymolysis at constant temperature, heating to raise the temperature and inactivate the enzyme, and cooling to obtain an enzymolysis liquid;
(2) sequentially taking 8-10 parts by weight of linoleic acid, 30-40 parts by weight of linseed oil, 2-4 parts by weight of carbodiimide and 100-150 parts by weight of enzymolysis liquid, adding the enzymolysis liquid into a reaction kettle, adjusting the pH to 3.2-3.4, adding the linoleic acid, the linseed oil and the carbodiimide, stirring at constant temperature for reaction, and concentrating under reduced pressure to obtain concentrated solution;
(3) according to the weight parts, sequentially taking 80-100 parts of concentrated solution, 8-10 parts of cosolvent, 3-5 parts of melamine, 0.1-0.2 part of ferric salt, 10-15 parts of filler and 1-3 parts of preservative, heating, stirring and mixing, adjusting the pH to 4.5-5.0, continuously stirring and mixing, and discharging to obtain the water-resistant soy protein adhesive.
The endopeptidase in the step (1) is any one of trypsin, chymotrypsin and elastase.
The cosolvent in the step (3) is prepared from glycerol and ethylene glycol according to a mass ratio of 10: 1-15: 1 is prepared by compounding.
And (3) the ferric salt is any one of ferric chloride, ferric nitrate or ferric sulfate.
And (4) the filler in the step (3) is any one of fumed silica or graphene oxide.
The preservative in the step (3) is any one of potassium sorbate, sodium benzoate, sodium dehydroacetate or butyl p-hydroxybenzoate.
The invention has the beneficial effects that:
(1) the technical scheme of the invention is that firstly endopeptidase is adopted to hydrolyze soybean protein, under the action of endopeptidase, the protein is primarily hydrolyzed, and is hydrolyzed from macromolecular protein into micromolecular polypeptide, so that the tertiary structure of the soybean protein is disintegrated, the number of active functional groups is increased, the reaction activity is improved, then linoleic acid is taken as a modifier, and is coupled to a polypeptide molecular chain through carbodiimide-mediated reaction, firstly, the linoleic acid molecular structure contains unsaturated carbon-carbon double bonds, so that the oxidation resistance of the product can be improved, secondly, long alkane chains in the linoleic acid molecular structure are exposed outside the polypeptide molecular structure, so that the water resistance of the outside of the polypeptide molecule is improved, and meanwhile, the structure is generated, so that the interface form compatibility of linseed oil and polypeptide is improved, the linseed oil is permeated into the inside of the polypeptide colloid structure, so that the linseed oil component occupies the position of partial functional groups inside the polypeptide colloid structure, the quantity of free radicals which can form hydrophilic bonds with water in the colloid is reduced, the water resistance in the colloid is synchronously improved, in addition, the linseed oil is dry oil, and the linseed oil is solidified in the bonding and solidifying process of a product, so that a linseed oil film with a hydrophobic structure is formed, and the water resistance of the product after solidification is further improved;
(2) the technical scheme of the invention is that firstly, through adding melamine and ferric salt, primary amino and secondary amino in the molecular structure of melamine can form hydrogen bond with oxygen-containing functional group (hydroxyl, carboxyl and the like) in inorganic filler, thereby being beneficial to the distribution of inorganic filler in an adhesive system, and the melamine can be used as a cross-linking agent to ensure that the protein after enzymolysis and activation is cross-linked again to form a new cross-linked network structure, thereby improving the adhesive strength of the adhesive product, and moreover, by adding the iron salt, iron ions ionized by the iron salt can be chelated with protein, thereby forming physical crosslinking in the protein, further improving the crosslinking network density, further improving the adhesive property, chelating iron ions and the protein, hydrophilic groups in protein molecules can be transferred to the inner side, and the problem that the water resistance is reduced because the hydrophilic groups are on the outer side after the product is cured is solved.
Detailed Description
Taking 20-30 parts of soybean protein, 2-4 parts of endopeptidase and 180-200 parts of water in sequence by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant temperature magnetic stirrer, stirring and mixing for 20-30 min at a constant temperature under the conditions that the temperature is 35-36 ℃ and the rotating speed is 400-800 r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 2-4 h at a constant temperature, heating to 90-95 ℃, keeping the temperature and inactivating enzyme for 10-20 min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 8-10 parts by weight of linoleic acid, 30-40 parts by weight of linseed oil, 2-4 parts by weight of carbodiimide and 100-150 parts by weight of enzymolysis liquid, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.2-3.4, adding the linoleic acid, the linseed oil and the carbodiimide after the pH adjustment is finished, stirring at a constant temperature for reaction for 4-6 hours under the conditions of the temperature of 65-70 ℃ and the rotating speed of 600-800 r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 30-40 minutes under the conditions of the temperature of 75-85 ℃ and the pressure of 500-520 kPa to obtain concentrated solution; according to the weight parts, 80-100 parts of concentrated solution, 8-10 parts of cosolvent, 3-5 parts of melamine, 0.1-0.2 part of ferric salt, 10-15 parts of filler and 1-3 parts of preservative are sequentially added into a mixer, heated, stirred and mixed for 2-3 hours at the rotating speed of 800-1200 r/min and at the temperature of 58-65 ℃, the pH of the materials in the mixer is adjusted to 4.5-5.0, and after the pH is adjusted, the materials are continuously stirred and mixed for 20-30 minutes, and then discharged, so that the water-resistant soy protein adhesive is obtained. The endopeptidase is any one of trypsin, chymotrypsin and elastase. The cosolvent is prepared from glycerol and glycol according to a mass ratio of 10: 1-15: 1 is prepared by compounding. The ferric salt is any one of ferric chloride, ferric nitrate or ferric sulfate. The filler is any one of fumed silica or graphene oxide. The preservative is any one of potassium sorbate, sodium benzoate, sodium dehydroacetate or butyl p-hydroxybenzoate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts of linoleic acid, 40 parts of linseed oil, 4 parts of carbodiimide and 150 parts of enzymolysis liquid according to parts by weight, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid, the linseed oil and the carbodiimide after the pH adjustment is finished, stirring and reacting for 6 hours at a constant temperature at the temperature of 70 ℃ and the rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating for 40 minutes under the conditions of the temperature of 85 ℃ and the pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of terminal peptidase 200 parts of water in sequence according to parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the terminal peptidase, continuously stirring and carrying out enzymolysis reaction for 4h at a constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts of linoleic acid, 40 parts of linseed oil, 4 parts of carbodiimide and 150 parts of enzymolysis liquid according to parts by weight, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid, the linseed oil and the carbodiimide after the pH adjustment is finished, stirring and reacting for 6 hours at a constant temperature at the temperature of 70 ℃ and the rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating for 40 minutes under the conditions of the temperature of 85 ℃ and the pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; taking 40 parts of linseed oil, 4 parts of carbodiimide and 150 parts of enzymolysis liquid in sequence according to parts by weight, firstly adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linseed oil and the carbodiimide after the pH adjustment is finished, then stirring and reacting for 6 hours at a constant temperature under the conditions of 70 ℃ and 800r/min of rotation speed, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 40 minutes under the conditions of 85 ℃ of temperature and 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; taking 10 parts by weight of linoleic acid, 4 parts by weight of carbodiimide and 150 parts by weight of enzymolysis liquid in turn, firstly adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid and the carbodiimide after the pH adjustment is finished, then stirring and reacting for 6 hours at a constant temperature under the conditions of a temperature of 70 ℃ and a rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 40 minutes under the conditions of a temperature of 85 ℃ and a pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; taking 10 parts by weight of linoleic acid, 40 parts by weight of linseed oil and 150 parts by weight of enzymolysis liquid in sequence, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid and the linseed oil after the pH is adjusted, stirring at a constant temperature for 6 hours at the temperature of 70 ℃ and the rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 40 minutes at the temperature of 85 ℃ and the pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts of linoleic acid, 40 parts of linseed oil, 4 parts of carbodiimide and 150 parts of enzymolysis liquid according to parts by weight, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid, the linseed oil and the carbodiimide after the pH adjustment is finished, stirring and reacting for 6 hours at a constant temperature at the temperature of 70 ℃ and the rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating for 40 minutes under the conditions of the temperature of 85 ℃ and the pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the materials in the mixer is adjusted to 5.0, the materials are continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soy protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts of linoleic acid, 40 parts of linseed oil, 4 parts of carbodiimide and 150 parts of enzymolysis liquid according to parts by weight, adding the enzymolysis liquid into a reaction kettle, adjusting the pH of the enzymolysis liquid in the reaction kettle to 3.4, adding the linoleic acid, the linseed oil and the carbodiimide after the pH adjustment is finished, stirring and reacting for 6 hours at a constant temperature at the temperature of 70 ℃ and the rotating speed of 800r/min, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating for 40 minutes under the conditions of the temperature of 85 ℃ and the pressure of 520kPa to obtain concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the materials in the mixer is adjusted to 5.0, the materials are continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soy protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts by weight of linoleic acid, 40 parts by weight of linseed oil, 4 parts by weight of carbodiimide and 150 parts by weight of enzymolysis liquid, adding the enzymolysis liquid into a reaction kettle, adding the linoleic acid, the linseed oil and the carbodiimide, stirring at a constant temperature and a rotation speed of 800r/min for reaction for 6 hours, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 40 minutes under the conditions of a temperature of 85 ℃ and a pressure of 520kPa to obtain a concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, the mixture is heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, the pH value of the material in the mixer is adjusted to 5.0, the mixture is continuously stirred and mixed for 30 minutes after the pH value is adjusted, and the water-resistant soybean protein adhesive is obtained after discharging. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Taking 30 parts of soybean protein and 4 parts of endopeptidase 200 parts of water in sequence according to the parts by weight, firstly mixing the soybean protein and the water, pouring the mixture into a No. 1 beaker, moving the No. 1 beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 30min at a constant temperature under the conditions that the temperature is 36 ℃ and the rotating speed is 800r/min, then adding the endopeptidase, continuously stirring and carrying out enzymolysis reaction for 4h at the constant temperature, heating to 95 ℃, keeping the temperature and inactivating the enzyme for 20min, naturally cooling to room temperature, and discharging to obtain an enzymolysis liquid; sequentially taking 10 parts by weight of linoleic acid, 40 parts by weight of linseed oil, 4 parts by weight of carbodiimide and 150 parts by weight of enzymolysis liquid, adding the enzymolysis liquid into a reaction kettle, adding the linoleic acid, the linseed oil and the carbodiimide, stirring at a constant temperature and a rotation speed of 800r/min for reaction for 6 hours, transferring the materials in the reaction kettle into a rotary evaporator, and concentrating under reduced pressure for 40 minutes under the conditions of a temperature of 85 ℃ and a pressure of 520kPa to obtain a concentrated solution; according to the weight parts, 100 parts of concentrated solution, 10 parts of cosolvent, 5 parts of melamine, 0.2 part of ferric salt, 15 parts of filler and 3 parts of preservative are sequentially added into a mixer, heated, stirred and mixed for 3 hours at the rotating speed of 1200r/min and the temperature of 65 ℃, continuously stirred and mixed for 30 minutes, and discharged, so that the water-resistant soy protein adhesive is obtained. The endopeptidase is trypsin. The cosolvent is prepared from glycerol and ethylene glycol according to a mass ratio of 15: 1 is prepared by compounding. The iron salt is ferric chloride. The filler is fumed silica. The preservative is potassium sorbate.
Comparative example: soy protein adhesive produced by science and technology limited, guangdong.
The water-resistant soy protein adhesives obtained in examples 1 to 9 and comparative products were subjected to performance tests, and the specific test methods were as follows:
the experimental board is a shaving board, the size specification is 250mm × 250mm × 10mm, glue is applied in a glue spraying mode, the glue application amount is 10% (the glue solid content accounts for absolutely dry shavings), a three-stage hot pressing process curve is adopted, the hot pressing pressure is 1.6MPa, the hot pressing temperature is 180 ℃, the hot pressing time is 9min, the prepared board is subjected to surface sanding treatment, and the dry internal gluing strength and the 2h water absorption thickness expansion rate of the board are measured, and the measuring method is shown in GB/T17657.
Specific detection results are shown in table 1:
TABLE 1 detection results of the performance of the water-resistant soy protein adhesive
As can be seen from the detection results in Table 1, the water-resistant soy protein adhesive prepared by the technical scheme of the invention has the characteristics of excellent water resistance and bonding strength, and has a wide prospect in the development of the chemical adhesive technology industry.
Claims (6)
1. A preparation method of a water-resistant soy protein adhesive is characterized by comprising the following specific preparation steps;
(1) taking 20-30 parts of soybean protein, 2-4 parts of endopeptidase and 180-200 parts of water in sequence by weight, firstly stirring and mixing the soybean protein and the water, then adding the endopeptidase, stirring and carrying out enzymolysis at constant temperature, heating to raise the temperature and inactivate the enzyme, and cooling to obtain an enzymolysis liquid;
(2) sequentially taking 8-10 parts by weight of linoleic acid, 30-40 parts by weight of linseed oil, 2-4 parts by weight of carbodiimide and 100-150 parts by weight of enzymolysis liquid, adding the enzymolysis liquid into a reaction kettle, adjusting the pH to 3.2-3.4, adding the linoleic acid, the linseed oil and the carbodiimide, stirring at constant temperature for reaction, and concentrating under reduced pressure to obtain concentrated solution;
(3) according to the weight parts, sequentially taking 80-100 parts of concentrated solution, 8-10 parts of cosolvent, 3-5 parts of melamine, 0.1-0.2 part of ferric salt, 10-15 parts of filler and 1-3 parts of preservative, heating, stirring and mixing, adjusting the pH to 4.5-5.0, continuously stirring and mixing, and discharging to obtain the water-resistant soy protein adhesive.
2. The method for preparing a water-resistant soy protein adhesive according to claim 1, wherein the endopeptidase in step (1) is any one of trypsin, chymotrypsin and elastase.
3. The preparation method of the water-resistant soy protein adhesive as claimed in claim 1, wherein the cosolvent in step (3) is prepared from glycerol and ethylene glycol in a mass ratio of 10: 1-15: 1 is prepared by compounding.
4. The preparation method of the water-resistant soy protein adhesive as claimed in claim 1, wherein the iron salt in step (3) is any one of ferric chloride, ferric nitrate or ferric sulfate.
5. The preparation method of the water-resistant soy protein adhesive according to claim 1, wherein the filler in step (3) is any one of fumed silica or graphene oxide.
6. The method for preparing a water-resistant soy protein adhesive as claimed in claim 1, wherein the preservative in step (3) is any one of potassium sorbate, sodium benzoate, sodium dehydroacetate or butyl p-hydroxybenzoate.
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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 |
| CN109439276B (en) * | 2018-11-23 | 2022-01-28 | 北京林业大学 | Formaldehyde-free soybean protein-based 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 |
| CN109517577B (en) * | 2018-11-23 | 2022-01-28 | 北京林业大学 | Tough soybean meal protein adhesive and preparation method thereof |
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