CN108342172A - A kind of preparation method of moisture-proof amylan - Google Patents
A kind of preparation method of moisture-proof amylan Download PDFInfo
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- CN108342172A CN108342172A CN201810199257.2A CN201810199257A CN108342172A CN 108342172 A CN108342172 A CN 108342172A CN 201810199257 A CN201810199257 A CN 201810199257A CN 108342172 A CN108342172 A CN 108342172A
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/02—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to polysaccharides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H1/00—Macromolecular products derived from proteins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention relates to technical field of adhesive preparation, and in particular to a kind of preparation method of moisture-proof amylan.The present invention obtains alkaline solution by raw material of soybean,Alkaline solution is placed in a centrifuge and is centrifugally separating to obtain supernatant liquor,Supernatant liquor is acidified with dilute hydrochloric acid to obtain lower layer's albumen precipitation,Take half albumen precipitation that sodium hydroxide solution is added,Obtain thermokalite protein degradation liquid,The other half albumen precipitation is handled to obtain the soyabean protein powder of acid heat processing,The soyabean protein powder that thermokalite protein degradation liquid and acid heat are handled mix and with starch-grafted styrene-acrylic emulsion Hybrid Heating,Obtain moisture-proof amylan,The present invention on starch by being grafted styrene-acrylic latex,The water suction effect of hydroxyl on starch can be shielded,To make amylan humidity resistance improve,Under higher hydrogen sodium hydroxide solution concentration alkali modification occurs for soybean protein,Part soybean protein hydrolyzes,The surface tension of gluing agent emulsion is caused to reduce,Contact angle increases,Achieve the effect that moisture-proof,It has a extensive future.
Description
Technical field
The present invention relates to technical field of adhesive preparation, and in particular to a kind of preparation method of moisture-proof amylan.
Background technology
Starch is a kind of natural macromolecule carbohydrate of polyhydroxy, have it is renewable, pollution-free, at low cost, can give birth to
The advantages that object is degraded.Amylan is using starch as natural adhesive made of base-material.Starch is that green plants passes through photosynthesis
The natural polymer of generation, so amylan belongs to plant glue.
The characteristics of amylan possesses abundance, and price is relatively low, easy to use, nonhazardous, is largely used to manufacture corrugated sheet
Carton, stamp gluing, timber processing, bookbinding etc. have good development prospect.But common amylan, by
In the limitation of structure itself, amylan poor water resistance, poor mechanical property, poor fluidity, slow drying speed, adhesive strength are poor,
So that it is promoted and use is restricted.But pure starch has many shortcomings, such as poor water resistance, mechanics as adhesive
Poor performance, poor fluidity, slow drying speed, adhesive strength are poor, and by physics or chemical method is needed to be modified it.
Over the past two years, someone carries out exploratory development to starch adhesive, using starch as primary raw material, progress acidolysis,
The processing such as oxidation, grafting, copolymerization and modification finally add certain auxiliary agent to prepare amylan, the amylan tool which prepares
Have the advantages that of low cost, environmentally friendly.Starch molecule C2、C3、C6On hydroxyl be easily oxidized, under different reaction conditions
Aldehyde radical, carbonyl, carboxyl are generated, obtained product is referred to as oxidized starch.Oxidized starch glues after physics and chemical modification
Initial bonding strength, rate of drying, stability of mixture etc. all have apparent improvement, but oxidized starch gluing compared with usual starch
The shortcomings of that there are intensity is low for agent, storage period is short and slow drying speed；Starch graft acrylic acid ester copolymer can effectively improve shallow lake
The adhesive strength and water resistance of powder adhesive, and the pernicious gases such as formaldehyde will not be released.However, the macromolecular chain of starch and
Heating could be gelatinized under the conditions of kernel structure causes starch only existing for a large amount of water, and consolidating for synthetic emulsion type adhesive contains
Measure that low and viscosity is big, be reflected in final synthetic product be exactly starch content it is relatively low；Acetate starch has than common starch
Better film forming, the transparency and glossiness of film are also preferable, and flexibility, extensibility, folding strength and abrasion resistance are high, and starch passes through
After peracetic acid esterification, acetyl group is introduced, intramolecular hydrogen bond is formd with the hydroxyl on glucose, hinders intermolecular hydrogen bonding
Generation and molecule aggregation, while enhance amylum adhesive anti -precipitability and improve bin stability.But single vinegar
Acid esters starch viscosity is high, and smear is poor.
Therefore, developing a kind of amylan that can solve above-mentioned performance issue is highly desirable.
Invention content
Present invention mainly solves the technical issues of, in current amylan preparation process, starch molecule C2、C3、C6On
Hydroxyl, which is easily oxidized, generates aldehyde radical, carbonyl, carboxyl, and obtained oxidized starch initial bonding strength enhances compared to pure amylan, still
The humidity resistance of oxidized starch is deteriorated, and content of starch declines, and cohesive force declines, and leads to the defect that degumming phenomenon occurs, provides
A kind of preparation method of moisture-proof amylan.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of moisture-proof amylan, it is characterised in that specifically preparation process is：
（1）Weigh 300~400g soybean and be placed in bean milling machine and grind, filtering removal fermented bean drink is sieved to obtain dregs of beans, by distilled water with
Dregs of beans mixes, and obtains dregs of beans suspension, and the pH of dregs of beans suspension is adjusted with sodium hydroxide solution, stirs, is alkalized at room temperature
Liquid,
（2）Alkaline solution is placed in a centrifuge centrifugation, isolated supernatant adjusts supernatant pH with hydrochloric acid, obtains acid
Change liquid, acidifying solution is placed in a centrifuge centrifugation, isolated lower layer's albumen precipitation；
（3）Sodium hydroxide solution and distilled water are added into three-necked flask, is slowly added into three-necked flask（1）Middle gained half
Albumen precipitation, heat temperature raising start blender and obtain reaction solution after insulated and stirred reaction, wait for that reaction solution is cooled to room temperature, add
Hydrochloric acid adjusts reaction solution pH, obtains thermokalite protein degradation liquid；
（4）By the other half albumen precipitation and mixed in hydrochloric acid, acidified protein liquid is obtained, acidified protein liquid is placed in high speed dispersor
Acidified protein liquid after dispersion is placed in baking oven, heat temperature raising by middle dispersion, dry, obtains the soyabean protein powder of acid heat processing；
（5）It counts in parts by weight, 20~30 parts of cornstarch, 0.5~0.8 part of ammonium persulfate and 70~80 parts of water is added to dress
It is mixed in the three-necked flask for having reflux condensing tube, blender and constant pressure funnel, water-bath, raising temperature, insulation reaction,
3~5 parts of sodium bicarbonates, 10~15 parts of styrene, 30~40 parts of butyl acrylates are added in cooling, and 1 is added dropwise with constant pressure funnel
~3 parts of potassium persulfate solutions after the reaction was continued, obtain starch-grafted styrene-acrylic emulsion；
（6）The soyabean protein powder that thermokalite protein degradation liquid and acid heat are handled is mixed, obtains egg mix white liquor, then will be starch-grafted
Styrene-acrylic emulsion is mixed with egg mix white liquor, and moisture-proof amylan is obtained after stirring.
Step（1）The distilled water is 10 ︰ 1 with dregs of beans mixing quality ratio, and the mass fraction of sodium hydroxide solution is 5%,
The pH that sodium hydroxide solution adjusts dregs of beans suspension is 8.5~9.5, and mixing time is 1.5~2.0h at room temperature.
Step（2）The centrifuge speed is 4000~5000r/mi, and the centrifugation time is 15~18min, hydrochloric acid
Mass fraction be 2%, it is 4.5~5.5 that hydrochloric acid, which adjusts supernatant liquor pH, and centrifugal rotational speed is 4000~5000r/ in centrifuge
min。
Step（3）The mass fraction of the sodium hydroxide solution is 25%, and temperature is 70~80 DEG C after heat temperature raising, is stirred
Mix rotating speed is 150~200r/min, and the insulated and stirred reaction time is 1.5~2.0h, add hydrochloric acid adjust reaction solution pH be 6.5~
7.0, obtain thermokalite protein degradation liquid.
Step（4）The mass fraction of the hydrochloric acid is 10%, the other half albumen precipitation is 1 ︰ with mixed in hydrochloric acid mass ratio
3, the rotating speed of high speed dispersor is 3000~4000r/min, and jitter time is 10~15min, and temperature is after baking oven heat temperature raising
To 120~125 DEG C, drying time is 0.5~1.0h.
Step（5）The bath temperature is 50~55 DEG C, and water-bath time is 45~55min, and temperature is after heating
90~100 DEG C, the insulation reaction time is 30~40min, and temperature is 80~85 DEG C after cooling, and potassium persulfate solution is in constant pressure addition
Drop rate in funnel is 3~5mL/min, and the mass fraction of potassium persulfate solution is 0.4%, the reaction was continued, and the time is 40~
50min。
Step（6）The mass ratio of the soyabean protein powder mixing of the thermokalite protein degradation liquid and acid heat processing is 6 ︰ 1, is formed sediment
The volume ratio that powder grafting styrene-acrylic emulsion is mixed with egg mix white liquor is 4 ︰ 1, and mixing time is 20~25min.
The beneficial effects of the invention are as follows：
（1）The present invention will be separated by filtration to obtain dregs of beans after soy beans, distilled water and dregs of beans be mixed to get using soybean as raw material
Dregs of beans suspension alkalizes to obtain alkaline solution by sodium hydroxide solution, alkaline solution is placed in a centrifuge, is centrifugally separating to obtain
Layer clear liquid, supernatant liquor is acidified with dilute hydrochloric acid, isolated lower layer's albumen precipitation takes half albumen precipitation that hydrogen is added thereto
Sodium hydroxide solution, heating and thermal insulation reaction, stirs to get reaction product, is adjusted to neutrality to obtain thermokalite drop after reaction product is cooled down
Protein liquid is solved, Centrifugal dispersion after the other half albumen precipitation is acidified is dried to obtain the soyabean protein powder of acid heat processing, corn is formed sediment
The mixing such as powder, sodium bicarbonate, styrene, butyl acrylate are added ammonium persulfate, the reaction of potassium persulfate solution initiation grafting, obtain
It is grafted styrene-acrylic emulsion to starch-grafted powder, the soyabean protein powder that thermokalite protein degradation liquid and acid heat are handled is mixed to get egg mix
Egg mix white liquor and starch-grafted styrene-acrylic emulsion Hybrid Heating are dispersed with stirring to obtain moisture-proof amylan, the present invention passes through by white liquor
It is grafted styrene-acrylic latex on starch, keeps branched hydroxy group of the amylan in preparation process substituted, under the hydroxy radical content aoxidized
Drop so that the water absorbing capacity of amylan reduces, and in addition grafting phenylpropyl polymers lipophilic is hydrophobic, can shield hydroxyl on starch
Absorb water effect, to make the humidity resistance of amylan be improved；
（2）The albumen extracted in soybean is modified by the present invention in the preparation process of moisture-proof amylan by acid heat, makes soybean egg
White strand is unfolded, and destroys the hydrogen bond of protein molecular, internal active group is exposed, taken in the modified soybean protein of acid heat
With multiple active sites, it is present in the micro oil phase of adhesive, active site can be connected with starch polymer chain, wherein starch
The skeleton for constituting adhesive improves water-soluble gluing in the modified soybean protein poorly water-soluble of surface of pressure-sensitive adhesive acid heat
Alkali modification occurs under higher hydrogen sodium hydroxide solution concentration for the water proofing property of agent, soybean protein, and part soybean protein hydrolyzes, will
Long chain amino acid is broken to small molecule peptide chain, and small molecule peptide chain has higher viscosity and more active groups, in active group
What cornstarch was aoxidized in group is more abundant, there is hydroxyl in starch polymer chain, and hydrophily is preferable, but monomer is thin after oxidation
Water substance, monomer are combined closer with soybean protein, and the surface tension of gluing agent emulsion is caused to reduce, and contact angle increases, gluing
The surface hydrophilicity of agent becomes very poor, moisture-proof to achieve the effect that, has a extensive future.
Specific implementation mode
It takes 300~400g soybean to be placed in bean milling machine to grind, dregs of beans is obtained by filtration, be in mass ratio with dregs of beans by distilled water
10 ︰ 1 are mixed, and obtain dregs of beans suspension, and the pH that the sodium hydroxide solution for being 5% with mass fraction adjusts dregs of beans suspension is 8.5~
9.5,1.5~2.0h is stirred at room temperature, obtains alkaline solution；Alkaline solution is placed in a centrifuge, with 4000~5000r/min rotating speeds
Centrifuge 15~18min, hydrochloric acid that isolated supernatant liquor is 2% with mass fraction adjust supernatant liquor pH be 4.5~
5.5, acidifying solution is obtained, acidifying solution is placed in a centrifuge, 15~18min is centrifuged with 4000~5000r/min rotating speeds, point
From obtaining lower layer's albumen precipitation；800~900mL mass fractions are added into three-necked flask as 25% sodium hydroxide solution, then to
The albumen precipitation of above-mentioned half is added in three-necked flask, is heated to 70~80 DEG C, starts blender, with 150~200r/min
Rotating speed obtain reaction product after insulated and stirred reacts 1.5~2.0h, wait for that reaction product is cooled to room temperature, add hydrochloric acid to adjust anti-
It is 6.5~7.0 to answer liquid pH, obtains thermokalite protein degradation liquid；The salt for being 10% with mass fraction by the other half remaining albumen precipitation
Acid is that 1 ︰ 3 is mixed in mass ratio, obtains acidified protein liquid, acidified protein liquid is placed in high speed dispersor, with 3000~
The rotating speed of 4000r/min disperses 10~15min, and the acidified protein liquid after dispersion is placed in baking oven, it is heated to 120~
125 DEG C, dry 0.5~1.0h obtains the soyabean protein powder of acid heat processing；Count in parts by weight, by 40~50 parts of cornstarch,
0.5~0.8 part of ammonium persulfate and 70~80 parts of water are added to three mouthfuls equipped with reflux condensing tube, blender and constant pressure funnel
In flask, 45~55min is reacted at 50~55 DEG C, increases temperature to 90~100 DEG C, continues 30~40min of insulation reaction, drop
Temperature is added 3~5 parts of sodium bicarbonates, 10~15 parts of styrene, 30~40 parts of butyl acrylates, uses constant pressure addition to 80~85 DEG C
The potassium persulfate solution that 1~3 part of mass fraction is 0.4% is added dropwise with the drop rate of 3~5mL/min for funnel, and the reaction was continued 40~
After 50min, starch-grafted styrene-acrylic emulsion is obtained；It is in mass ratio by the soyabean protein powder that thermokalite protein degradation liquid and acid heat are handled
6 ︰ 1 are mixed, and are obtained egg mix white liquor, then starch-grafted styrene-acrylic emulsion is mixed for 4 ︰ 1 by volume with egg mix white liquor, are heated
It is warming up to 40~50min, moisture-proof amylan is obtained after being dispersed with stirring 20~25min.
Example 1
It takes 300g soybean to be placed in bean milling machine to grind, dregs of beans is obtained by filtration, distilled water is mixed for 10 ︰ 1 in mass ratio with dregs of beans,
Dregs of beans suspension is obtained, the pH that the sodium hydroxide solution for being 5% with mass fraction adjusts dregs of beans suspension is 8.5, is stirred at room temperature
1.5h obtains alkaline solution；Alkaline solution is placed in a centrifuge, with 4000r/min rotating speeds centrifuge 15min, it is isolated on
Layer clear liquid, it is 4.5 that the hydrochloric acid for being 2% with mass fraction, which adjusts supernatant liquor pH, obtains acidifying solution, acidifying solution is placed in centrifuge
In, 15min, isolated lower layer's albumen precipitation are centrifuged with 4000r/min rotating speeds；800mL matter is added into three-necked flask
The sodium hydroxide solution that score is 25% is measured, then the albumen precipitation of above-mentioned half is added to three-necked flask, is heated to 70 DEG C,
Start blender, obtains reaction product after insulated and stirred reacts 1.5h with the rotating speed of 150r/min, wait for that reaction product is cooled to
Room temperature, it is 6.5 to add hydrochloric acid to adjust reaction solution pH, obtains thermokalite protein degradation liquid；By the other half remaining albumen precipitation and quality
The hydrochloric acid that score is 10% is 1 ︰ 3 mixing in mass ratio, obtains acidified protein liquid, acidified protein liquid is placed in high speed dispersor,
Disperse 10min with the rotating speed of 3000r/min, the acidified protein liquid after dispersion is placed in baking oven, is heated to 120 DEG C, does
Dry 0.5h obtains the soyabean protein powder of acid heat processing；It counts in parts by weight, by 40 parts of cornstarch, 0.5 part of ammonium persulfate and 70
Part water is added in the three-necked flask equipped with reflux condensing tube, blender and constant pressure funnel, reacts 45min at 50 DEG C,
Temperature is increased to 90 DEG C, continues insulation reaction 30min, is cooled to 80 DEG C, be added 3 parts of sodium bicarbonates, 10 parts of styrene, 30 part third
Olefin(e) acid butyl ester, it is molten for 0.4% potassium peroxydisulfate with drop rate 1 part of mass fraction of dropwise addition of 3mL/min with constant pressure funnel
Liquid after the reaction was continued 40min, obtains starch-grafted styrene-acrylic emulsion；The soybean protein that thermokalite protein degradation liquid and acid heat are handled
Powder is that 6 ︰ 1 are mixed in mass ratio, obtains egg mix white liquor, then be by volume by starch-grafted styrene-acrylic emulsion and egg mix white liquor
4 ︰ 1 are mixed, and are heated to 40min, moisture-proof amylan is obtained after being dispersed with stirring 20min.
Example 2
It takes 350g soybean to be placed in bean milling machine to grind, dregs of beans is obtained by filtration, distilled water is mixed for 10 ︰ 1 in mass ratio with dregs of beans,
Dregs of beans suspension is obtained, the pH that the sodium hydroxide solution for being 5% with mass fraction adjusts dregs of beans suspension is 9.0, is stirred at room temperature
1.7h obtains alkaline solution；Alkaline solution is placed in a centrifuge, with 4500r/min rotating speeds centrifuge 17min, it is isolated on
Layer clear liquid, it is 5.0 that the hydrochloric acid for being 2% with mass fraction, which adjusts supernatant liquor pH, obtains acidifying solution, acidifying solution is placed in centrifuge
In, 16min, isolated lower layer's albumen precipitation are centrifuged with 4500r/min rotating speeds；850mL matter is added into three-necked flask
The sodium hydroxide solution that score is 25% is measured, then the albumen precipitation of above-mentioned half is added to three-necked flask, is heated to 75 DEG C,
Start blender, obtains reaction product after insulated and stirred reacts 1.6h with the rotating speed of 175r/min, wait for that reaction product is cooled to
Room temperature, it is 6.7 to add hydrochloric acid to adjust reaction solution pH, obtains thermokalite protein degradation liquid；By the other half remaining albumen precipitation and quality
The hydrochloric acid that score is 10% is 1 ︰ 3 mixing in mass ratio, obtains acidified protein liquid, acidified protein liquid is placed in high speed dispersor,
Disperse 13min with the rotating speed of 3500r/min, the acidified protein liquid after dispersion is placed in baking oven, is heated to 123 DEG C, does
Dry 0.7h obtains the soyabean protein powder of acid heat processing；It counts in parts by weight, by 45 parts of cornstarch, 0.7 part of ammonium persulfate and 75
Part water is added in the three-necked flask equipped with reflux condensing tube, blender and constant pressure funnel, reacts 50min at 53 DEG C,
Temperature is increased to 95 DEG C, continues insulation reaction 35min, is cooled to 83 DEG C, be added 4 parts of sodium bicarbonates, 13 parts of styrene, 35 part third
Olefin(e) acid butyl ester, it is molten for 0.4% potassium peroxydisulfate with drop rate 2 parts of mass fractions of dropwise addition of 4mL/min with constant pressure funnel
Liquid after the reaction was continued 45min, obtains starch-grafted styrene-acrylic emulsion；The soybean protein that thermokalite protein degradation liquid and acid heat are handled
Powder is that 6 ︰ 1 are mixed in mass ratio, obtains egg mix white liquor, then be by volume by starch-grafted styrene-acrylic emulsion and egg mix white liquor
4 ︰ 1 are mixed, and are heated to 45min, moisture-proof amylan is obtained after being dispersed with stirring 23min.
Example 3
It takes 400g soybean to be placed in bean milling machine to grind, dregs of beans is obtained by filtration, distilled water is mixed for 10 ︰ 1 in mass ratio with dregs of beans,
Dregs of beans suspension is obtained, the pH that the sodium hydroxide solution for being 5% with mass fraction adjusts dregs of beans suspension is 9.5, is stirred at room temperature
2.0h obtains alkaline solution；Alkaline solution is placed in a centrifuge, with 5000r/min rotating speeds centrifuge 18min, it is isolated on
Layer clear liquid, it is 5.5 that the hydrochloric acid for being 2% with mass fraction, which adjusts supernatant liquor pH, obtains acidifying solution, acidifying solution is placed in centrifuge
In, 18min, isolated lower layer's albumen precipitation are centrifuged with 5000r/min rotating speeds；900mL matter is added into three-necked flask
The sodium hydroxide solution that score is 25% is measured, then the albumen precipitation of above-mentioned half is added to three-necked flask, is heated to 80 DEG C,
Start blender, obtains reaction product after insulated and stirred reacts 2.0h with the rotating speed of 200r/min, wait for that reaction product is cooled to
Room temperature, it is 7.0 to add hydrochloric acid to adjust reaction solution pH, obtains thermokalite protein degradation liquid；By the other half remaining albumen precipitation and quality
The hydrochloric acid that score is 10% is 1 ︰ 3 mixing in mass ratio, obtains acidified protein liquid, acidified protein liquid is placed in high speed dispersor,
Disperse 15min with the rotating speed of 4000r/min, the acidified protein liquid after dispersion is placed in baking oven, is heated to 120~125
DEG C, dry 1.0h obtains the soyabean protein powder of acid heat processing；It counts in parts by weight, by 50 parts of cornstarch, 0.8 part of persulfuric acid
Ammonium and 80 parts of water are added in the three-necked flask equipped with reflux condensing tube, blender and constant pressure funnel, are reacted at 55 DEG C
55min increases temperature to 100 DEG C, continues insulation reaction 40min, be cooled to 85 DEG C, 5 parts of sodium bicarbonates, 15 parts of benzene second are added
The mistake that 3 parts of mass fractions are 0.4% is added dropwise with the drop rate of 5mL/min with constant pressure funnel in alkene, 40 parts of butyl acrylates
Potassium sulfate solution after the reaction was continued 50min, obtains starch-grafted styrene-acrylic emulsion；Thermokalite protein degradation liquid and acid heat are handled
Soyabean protein powder is that 6 ︰ 1 are mixed in mass ratio, obtains egg mix white liquor, then starch-grafted styrene-acrylic emulsion and egg mix white liquor are pressed
Volume ratio mixes for 4 ︰ 1, is heated to 50min, moisture-proof amylan is obtained after being dispersed with stirring 25min.
Comparative example
With the amylan of company of Jining City production as a comparison case in moisture-proof amylan produced by the present invention and comparative example
Amylan is detected, and testing result is as shown in table 1：
1, solid content
Reference standard GB/T14074-2006《Based Wood Adhesives and its resin method of inspection》It is tested.
2, wet shape bonding strength
Reference standard GB/T17657-2013《Strength of Plywood measures》It is tested.
1 performance measurement result of table
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Solid content（%） | 39.8 | 40.8 | 42.7 | 25.0 |
| The just glutinous time（s） | 25 | 23 | 20 | 48 |
| Viscosity（mPa·s） | 85234 | 85342 | 85384 | 53942 |
| Wet shape bonding strength（MPa） | 0.98 | 0.99 | 1.02 | 0.71 |
| Resistance to room temperature is aqueous（h） | >350 | >350 | >350 | >200 |
| It is resistance to cold aqueous（h） | >500 | >500 | >500 | >300 |
According to data in table 1 it is found that moisture-proof amylan produced by the present invention, has water-tolerant, high mechanical properties, mobility
Well, the advantages that rate of drying is fast, adhesive strength is high, greatly reduces cost, safety and environmental protection, hence it is evident that is better than comparative example.Cause
This, has wide prospect of the application.
Claims (7)
1. a kind of preparation method of moisture-proof amylan, it is characterised in that specifically preparation process is：
（1）Weigh 300~400g soybean and be placed in bean milling machine and grind, filtering removal fermented bean drink is sieved to obtain dregs of beans, by distilled water with
Dregs of beans mixes, and obtains dregs of beans suspension, and the pH of dregs of beans suspension is adjusted with sodium hydroxide solution, stirs, is alkalized at room temperature
Liquid；
（2）Alkaline solution is placed in a centrifuge centrifugation, isolated supernatant adjusts supernatant pH with hydrochloric acid, obtains acid
Change liquid, acidifying solution is placed in a centrifuge centrifugation, isolated lower layer's albumen precipitation；
（3）Sodium hydroxide solution and distilled water are added into three-necked flask, is slowly added into three-necked flask（1）Middle gained half
Albumen precipitation, heat temperature raising, start blender, insulated and stirred reaction after, obtain reaction solution, wait for that reaction solution is cooled to room temperature,
Add hydrochloric acid to adjust reaction solution pH, obtains thermokalite protein degradation liquid；
（4）By the other half albumen precipitation and mixed in hydrochloric acid, acidified protein liquid is obtained, acidified protein liquid is placed in high speed dispersion
Disperse in machine, the acidified protein liquid after dispersion is placed in baking oven, heat temperature raising, it is dry, obtain the soybean protein of acid heat processing
Powder；
（5）It counts in parts by weight, 20~30 parts of cornstarch, 0.5~0.8 part of ammonium persulfate and 70~80 parts of water is added to
It is mixed in three-necked flask equipped with reflux condensing tube, blender and constant pressure funnel, water-bath, increases temperature, heat preservation is anti-
It answers, cools down, 3~5 parts of sodium bicarbonates, 10~15 parts of styrene, 30~40 parts of butyl acrylates are added, are dripped with constant pressure funnel
Add 1~3 part of potassium persulfate solution, after the reaction was continued, obtain starch-grafted styrene-acrylic emulsion；
（6）The soyabean protein powder that thermokalite protein degradation liquid and acid heat are handled is mixed, obtains egg mix white liquor, then will be starch-grafted
Styrene-acrylic emulsion is mixed with egg mix white liquor, and moisture-proof amylan is obtained after stirring.
2. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（1）The steaming
Distilled water is 10 ︰ 1 with dregs of beans mixing quality ratio, and the mass fraction of sodium hydroxide solution is 5%, and it is outstanding that sodium hydroxide solution adjusts dregs of beans
The pH of supernatant liquid is 8.5~9.5, and mixing time is 1.5~2.0h at room temperature.
3. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（2）It is described from
Scheming rotating speed is 4000~5000r/mi, and the centrifugation time is 15~18min, and the mass fraction of hydrochloric acid is 2%, and hydrochloric acid is adjusted
Supernatant liquor pH is 4.5~5.5, and centrifugal rotational speed is 4000~5000r/min in centrifuge.
4. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（3）The hydrogen
The mass fraction of sodium hydroxide solution is 25%, and temperature is 70~80 DEG C after heat temperature raising, and speed of agitator is 150~200r/min, is protected
Temperature is stirred to react the time as 1.5~2.0h, and it is 6.5~7.0 to add hydrochloric acid to adjust reaction solution pH, obtains thermokalite protein degradation liquid.
5. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（4）The salt
The mass fraction of acid is 10%, the other half albumen precipitation is 1 ︰ 3 with mixed in hydrochloric acid mass ratio, and the rotating speed of high speed dispersor is
3000~4000r/min, jitter time are 10~15min, and temperature is the drying time to 120~125 DEG C after baking oven heat temperature raising
For 0.5~1.0h.
6. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（5）The water
Bath temperature is 50~55 DEG C, and water-bath time is 45~55min, and temperature is 90~100 DEG C after heating, and the insulation reaction time is
30~40min, after cooling temperature be 80~85 DEG C, drop rate of the potassium persulfate solution in constant pressure funnel be 3~
The mass fraction of 5mL/min, potassium persulfate solution are 0.4%, and the reaction was continued, and the time is 40~50min.
7. a kind of preparation method of moisture-proof amylan according to claim 1, it is characterised in that：Step（6）The heat
The mass ratio of the soyabean protein powder mixing of alkaline degradation protein liquid and acid heat processing is 6 ︰ 1, starch-grafted styrene-acrylic emulsion and egg mix
The volume ratio of white liquor mixing is 4 ︰ 1, and mixing time is 20~25min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109049202A (en) * | 2018-08-29 | 2018-12-21 | 佛山市森昂生物科技有限公司 | A kind of method of timber anticracking |
| CN109624019A (en) * | 2019-01-17 | 2019-04-16 | 吕旭光 | A kind of disposable tableware and manufacture craft |
| CN110128978A (en) * | 2019-04-30 | 2019-08-16 | 龙海燕 | A kind of preparation method of electrostatic spinning adhesive |
| CN110484193A (en) * | 2019-08-28 | 2019-11-22 | 韦权 | A kind of preparation method of the moisture-proof glass cement of high cohesive force |
| CN112266492A (en) * | 2020-11-21 | 2021-01-26 | 蚌埠市维光塑胶制品有限公司 | Preparation method of hydrophobic film with low water absorption |
| CN116284899A (en) * | 2023-01-17 | 2023-06-23 | 哈尔滨商业大学 | Preparation method of soybean protein isolate composite membrane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103180137A (en) * | 2010-10-27 | 2013-06-26 | 罗盖特公司 | Method for producing a multilayer structure comprising an adhesive composition based on an amylaceous material |
| CN104497965A (en) * | 2015-01-26 | 2015-04-08 | 东北林业大学 | Waterproof-level soy protein adhesive and preparation method thereof |
| CN107619648A (en) * | 2017-08-09 | 2018-01-23 | 无锡海特新材料研究院有限公司 | A kind of St/BA modifications by copolymerization oxidized starch adhesive, and preparation method thereof |
-
2018
- 2018-03-12 CN CN201810199257.2A patent/CN108342172A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103180137A (en) * | 2010-10-27 | 2013-06-26 | 罗盖特公司 | Method for producing a multilayer structure comprising an adhesive composition based on an amylaceous material |
| CN104497965A (en) * | 2015-01-26 | 2015-04-08 | 东北林业大学 | Waterproof-level soy protein adhesive and preparation method thereof |
| CN107619648A (en) * | 2017-08-09 | 2018-01-23 | 无锡海特新材料研究院有限公司 | A kind of St/BA modifications by copolymerization oxidized starch adhesive, and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱伍权: "大豆蛋白的化学交联改性及其对大豆木材胶黏剂性能的影响", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109049202A (en) * | 2018-08-29 | 2018-12-21 | 佛山市森昂生物科技有限公司 | A kind of method of timber anticracking |
| CN109624019A (en) * | 2019-01-17 | 2019-04-16 | 吕旭光 | A kind of disposable tableware and manufacture craft |
| CN110128978A (en) * | 2019-04-30 | 2019-08-16 | 龙海燕 | A kind of preparation method of electrostatic spinning adhesive |
| CN110484193A (en) * | 2019-08-28 | 2019-11-22 | 韦权 | A kind of preparation method of the moisture-proof glass cement of high cohesive force |
| CN112266492A (en) * | 2020-11-21 | 2021-01-26 | 蚌埠市维光塑胶制品有限公司 | Preparation method of hydrophobic film with low water absorption |
| CN116284899A (en) * | 2023-01-17 | 2023-06-23 | 哈尔滨商业大学 | Preparation method of soybean protein isolate composite membrane |
| CN116284899B (en) * | 2023-01-17 | 2023-10-20 | 哈尔滨商业大学 | Preparation method of soybean protein isolate composite membrane |
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