CN108659751A - A kind of preparation method of modified corn starch adhesive - Google Patents
A kind of preparation method of modified corn starch adhesive Download PDFInfo
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- CN108659751A CN108659751A CN201810567956.8A CN201810567956A CN108659751A CN 108659751 A CN108659751 A CN 108659751A CN 201810567956 A CN201810567956 A CN 201810567956A CN 108659751 A CN108659751 A CN 108659751A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
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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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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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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- 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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The present invention relates to a kind of preparation methods of modified corn starch adhesive, belong to field of adhesive technology.The present invention prepares the obtained oxidised maize starch of cornstarch as primary raw material using the composite oxidant that hydrogen peroxide and potassium peroxydisulfate mix, and oxidized starch is compared with native starch, has good fluidity, viscosity stability is high, the advantages that permeability is strong, and cohesive force is good, the composite oxidant that the hydrogen peroxide and potassium peroxydisulfate of selection mix, stability is good, more thoroughly, remaining oxidant content is few in colloid for oxidation reaction ratio, and tack is good, rate of drying is fast, and pollution is small；The method that the present invention uses free-radical emulsion polymerization is added organosilicon and is modified to starch, and the adhesion strength of starch adhesive obtained, water resistance are relatively preferable, reach preparation simple, clean environment firendly, function admirable and it is at low cost the purpose of；A small amount of tbp is added in the present invention, effectively prevents that the bubble generated when paste agent gelatinization is added.
Description
Technical field
The present invention relates to a kind of preparation methods of modified corn starch adhesive, belong to field of adhesive technology.
Background technology
With being constantly progressive for science and technology, every profession and trade is higher and higher to the performance requirement of adhesive.How gluing is reduced
Agent cost, the project for person's common concern that raising Adhensive performance becomes chemical research.
Currently, the adhesive used on domestic market mainly has casein glue, chemical glue, amylan and their improvement
Glue.Can be seen that casein glue in various performances by the comparison of performance, performance is preferable, but casein glue raw material is rare, valence
Lattice are expensive, it is difficult to as the glue kind of large-scale use.For chemical glue due to its toxicity and high pollution, use is also restrained.It forms sediment
Powder raw material is cheap and easily-available, nontoxic and pollution-free, but the glueability existing defects of ative starch, generally requires and is used after being modified.
Modified starch adhesive has increasingly been valued by people as universal natural adhesive.This is mainly based upon
Following two reasons：First, starch is a kind of resourceful, cheap, widely used natural macromolecular material, there is nothing
Poison, free from extraneous odour, free of contamination advantage.Second is that with the increasingly reduction of petroleum resources, give the chemical adhesive that oil is raw material
Threat is constituted, to promote domestic and international research worker competitively to find substitute, starch adhesive causes people's again
Interest.Modified starch adhesive has been widely used in numerous industry such as corrugated case, construction material, artificial cardboard and label
Field.
Adhesive is since 1958 in China's large-scale production.The nineties in last century, the glue of World Developed Countries
Stick industry enters high speed development stage, annual average rate of increase 3%, and China has then reached 9.5%, becomes China's chemical field
One of industry with fastest developing speed.As economic is constantly progressive, adhesive industry is increasingly valued by people.
Currently, the application of adhesive has penetrated into each department of national economy, including clothes, light industry, aerospace,
The various fields such as food packaging, health care.More stringent requirements are proposed for this production to adhesive, and current domestic adhesive
It is insufficient to there is both sides in industry：First, industry level is not high, the technological element of a product is low；Second is that non-environmental protection product accounts for mainstream, it is high
Performance environment-friendly products rely primarily on import.Therefore, it is necessary to select a kind of nothing
Pollution, reproducible material continuously improve production technology, increase technology content, develop high performance as raw material
Adhesive kind.
Starch is non-toxic and tasteless, good film-forming property and has good adhesive property, complete in certain fields after modified
Seriously polluted chemical glue and expensive into chewing-gum can be substituted entirely, therefore is paid close attention to by numerous chemical research persons.With
Going deep into for starch adhesive research, various new method of modifying and preparation process will continue to bring out, and kind and performance will
It is continuously increased and improves, the application range of starch adhesive also can constantly be extended.
Invention content
The technical problems to be solved by the invention：For existing corn starch adhesive drying time is long, adhesion strength is low
The problem of, provide a kind of preparation method of modified corn starch adhesive.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；
（2）The cornstarch emulsion that mass fraction is 40% is prepared, the salt acid for adjusting pH for being 3% with mass fraction is to 3~5, then presses
Parts by weight meter weighs 50~60 parts of modified corn starch lotions, 0.1~0.3 part of copper sulphate and 1~3 part of composite oxygen respectively
Agent is placed in three-necked flask, is stirred and is placed in 1~2h of heating water bath at 45~55 DEG C, obtains reaction solution and in reaction solution
10% sodium sulfite solution of mass fraction of dropwise reaction liquid quality 2%, standing are cooled to room temperature, and obtain mixed phase, filter to obtain filter
Slag, is washed with water filter residue 1~2 time, is dried in 50~60 DEG C of baking ovens, crushes, obtains oxidised maize starch, take oxidised maize starch
And mixed with deionized water, it is configured to the corn starch milk of mass fraction 30%；
（3）It counts in parts by weight, respectively 30% corn starch milk of 40~50 parts of weighing, 6~8 parts of sodium hydroxides, 0.1~0.3
The tributyl phosphate, 0.1~0.2 part of ethylene glycol, 0.5~0.7 part of polyvinyl alcohol of part（Mass fraction is 10%）, 0.2~
0.4 part of ammonium persulfate, 10~14 parts of acrylamide and 5~6 parts of vinyl silane triisopropoxide, in four-hole boiling flask
30% corn starch milk is added, under 45~55 DEG C of water-baths, stirs 10~20min, is warming up to 85~90 DEG C, hydroxide is added
Sodium is gelatinized 20~30min, is subsequently cooled to 45~55 DEG C, be added tributyl phosphate, ethylene glycol and mass fraction be 10% it is poly-
Vinyl alcohol after leading to 4~8min of nitrogen, starts that ammonium persulfate and acrylamide is added dropwise, and control drips off in 3~4h, when grafting is anti-
After should carrying out 1.5~2h, starting that vinyl silane triisopropoxide is added dropwise, control drips off in 1~2h, 4~5h of graft copolymerization,
It is cooled to room temperature up to corn starch adhesive；
（4）It counts in parts by weight, weighs 6~8 parts of Nano-meter SiO_2 respectively2, 40~50 parts by weight absolute ethyl alcohol/water（Volume ratio
For 3 ︰ 1）, 2~3 parts of 0.2%~0.3% silane coupling agent, by Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water,
Keep its fully dispersed under 4000r/min high speed shears, adjusts shear rate to 2000r/min, 65~75 DEG C of left sides of reaction temperature
0.2%~0.3% silane coupling agent is added in the right side, with oxalic acid solution regulation system pH value to 3~5, is obtained after reacting 90~100min
Suspension, filters to obtain filter cake, and filter cake puts dry 1~2h under 80 DEG C of baking ovens, is cooled to room temperature and grinds to get modified Nano SiO2
Powder；
（5）It counts in parts by weight, weighs 4~5 parts of modified Nano SiO respectively2Powder, 20~30 parts by weight Corn starch gluings
Agent, by modified Nano SiO at 45~55 DEG C of ultrasonic device2Powder is slowly added in corn starch adhesive, is added and is persistently shaken
1~2h is swung to get modified corn starch adhesive.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention prepares the obtained oxidation of cornstarch with the composite oxidant that hydrogen peroxide and potassium peroxydisulfate mix
Cornstarch is primary raw material, and oxidized starch is compared with native starch, has good fluidity, and viscosity stability is high, and permeability is strong,
The advantages that cohesive force is good, the composite oxidant that the hydrogen peroxide and potassium peroxydisulfate of selection mix, stability is good, oxidation reaction
Than more thoroughly, remaining oxidant content is few in colloid, tack is good, and rate of drying is fast, and pollution is small；
（2）The method that the present invention uses free-radical emulsion polymerization is added organosilicon and is modified to starch, starch gluing obtained
The adhesion strength of agent, water resistance are relatively preferable, reach preparation simple, clean environment firendly, function admirable and it is at low cost the purpose of；This
A small amount of tbp is added in invention, effectively prevents that the bubble generated when paste agent gelatinization is added；
（3）Nano-meter SiO_22Exist typically in the form of aggregate, therefore, before being added in corn starch adhesive, it is necessary to
Make surface modification treatment, the silane coupling agent that the present invention uses carries out surface modification treatment to it, keeps nano particle full and uniform
Ground disperses, and makes it easier to be distributed in corn starch adhesive；
（4）The present invention uses modified Nano SiO2Particle size is small, and surface atom number is more, and surface is seriously coordinated deficiency, Yi Yuyu
Oxygen in rice starch adhesive plays bonding action, improves intermolecular bonding force, while modified Nano SiO2Molecule is three-dimensional chain
Structure, there are the hydroxyls of different bond styles on surface, may be cross-linked into big point with the hydroxyl reaction in corn starch adhesive
Son, to make water-fast, heat-resisting, bin stability improve.
Specific implementation mode
In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；It is 40% to prepare mass fraction
Cornstarch emulsion, with mass fraction be 3% salt acid for adjusting pH counted to 3~5, then in parts by weight, respectively weigh 50~60
Part modified corn starch lotion, 0.1~0.3 part of copper sulphate and 1~3 part of composite oxidant are placed in three-necked flask, and stirring is mixed
Merging is placed in 1~2h of heating water bath at 45~55 DEG C, obtains reaction solution and to the quality of dropwise reaction liquid quality 2% in reaction solution point
Several 10% sodium sulfite solutions, standing are cooled to room temperature, and obtain mixed phase, filter to obtain filter residue, filter residue are washed with water 1~2 time, 50
It is dried in~60 DEG C of baking ovens, crushes, obtain oxidised maize starch, take oxidised maize starch and mixed with deionized water, be configured to matter
Measure the corn starch milk of score 30%；It counts in parts by weight, respectively 30% corn starch milk, 6~8 parts of hydrogen of 40~50 parts of weighing
Sodium oxide molybdena, 0.1~0.3 part of tributyl phosphate, 0.1~0.2 part of ethylene glycol, 0.5~0.7 part of polyvinyl alcohol（Quality point
Number is 10%）, 0.2~0.4 part of ammonium persulfate, 10~14 parts of acrylamide and 5~6 parts of three isopropoxy silicon of vinyl
30% corn starch milk is added in alkane in four-hole boiling flask, under 45~55 DEG C of water-baths, stirs 10~20min, it is warming up to 85~
90 DEG C, sodium hydroxide is added, is gelatinized 20~30min, is subsequently cooled to 45~55 DEG C, tributyl phosphate, ethylene glycol and matter is added
The polyvinyl alcohol that score is 10% is measured, after leading to 4~8min of nitrogen, starts that ammonium persulfate and acrylamide is added dropwise, controls in 3~4h
It inside drips off, after graft reaction carries out 1.5~2h, starts that vinyl silane triisopropoxide is added dropwise, control is dripped in 1~2h
Complete, 4~5h of graft copolymerization is cooled to room temperature up to corn starch adhesive；It counts in parts by weight, weighing 6~8 parts respectively receives
Rice SiO2, 40~50 parts by weight absolute ethyl alcohol/water（Volume ratio is 3 ︰ 1）, 2~3 parts of 0.2%~0.3% silane coupling agent,
By Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water, keeps its fully dispersed under 4000r/min high speed shears, adjust
0.2%~0.3% silane coupling agent is added in shear rate to 2000r/min, 65~75 DEG C or so of reaction temperature, molten with oxalic acid
Liquid regulation system pH value obtains suspension to 3~5 after reacting 90~100min, filters to obtain filter cake, and filter cake is put dry under 80 DEG C of baking ovens
1~2h is cooled to room temperature and is ground to get modified Nano SiO2Powder；It counts in parts by weight, weighs 4~5 parts of modification respectively
Nano-meter SiO_22Powder, 20~30 parts by weight Corn starch adhesive, by modified Nano SiO at 45~55 DEG C of ultrasonic device2Powder
It is slowly added in corn starch adhesive, adds 1~2h of persistent oscillation to get modified corn starch adhesive.
In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；It is 40% to prepare mass fraction
Cornstarch emulsion, with mass fraction be 3% salt acid for adjusting pH counted to 3, then in parts by weight, respectively weigh 50 parts of modifications
Cornstarch emulsion, 0.1 part of copper sulphate and 1 part of composite oxidant are placed in three-necked flask, are stirred and are placed at 45 DEG C
Heating water bath 1h, obtains reaction solution and to 10% sodium sulfite solution of mass fraction of dropwise reaction liquid quality 2% in reaction solution, quiet
It sets and is cooled to room temperature, obtain mixed phase, filter to obtain filter residue, filter residue is washed with water 1 time, dried in 50 DEG C of baking ovens, crush, must aoxidize
Cornstarch takes oxidised maize starch and is mixed with deionized water, is configured to the corn starch milk of mass fraction 30%；By weight
Number meter, respectively weigh 40 parts 30% corn starch milk, 6 parts of sodium hydroxides, 0.1 part of tributyl phosphate, 0.1 part of second
Glycol, 0.5 part of polyvinyl alcohol（Mass fraction is 10%）, 0.2 part of ammonium persulfate, 10 parts of acrylamide and 5 parts of ethylene
30% corn starch milk is added in three isopropoxy silane of base in four-hole boiling flask, under 45 DEG C of water-baths, stirs 10min, heating
To 85 DEG C, sodium hydroxide is added, is gelatinized 20min, is subsequently cooled to 45 DEG C, tributyl phosphate, ethylene glycol and mass fraction is added
For 10% polyvinyl alcohol, after leading to nitrogen 4min, start that ammonium persulfate and acrylamide is added dropwise, control drips off in 3h, works as grafting
After reaction carries out 1.5h, start that vinyl silane triisopropoxide is added dropwise, control drips off in 1h, and graft copolymerization 4h is cooled to
Room temperature is up to corn starch adhesive；It counts in parts by weight, weighs 6 parts of Nano-meter SiO_2 respectively2, 40 parts by weight absolute ethyl alcohol/
Water（Volume ratio is 3 ︰ 1）, 2 parts of 0.2% silane coupling agent, by Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water,
Keep its fully dispersed under 4000r/min high speed shears, adjusts shear rate to 2000r/min, 65 DEG C or so of reaction temperature adds
The silane coupling agent for entering 0.2% is obtained suspension after reacting 90min, is filtered to obtain filter cake with oxalic acid solution regulation system pH value to 3,
Filter cake puts dry 1h under 80 DEG C of baking ovens, is cooled to room temperature and grinds to get modified Nano SiO2Powder；It counts in parts by weight, point
Also known as measure 4 parts of modified Nano SiO2Powder, 20 parts by weight Corn starch adhesive, by modified Nano at 45 DEG C of ultrasonic device
SiO2Powder is slowly added in corn starch adhesive, adds persistent oscillation 1h to get modified corn starch adhesive.
In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；It is 40% to prepare mass fraction
Cornstarch emulsion, with mass fraction be 3% salt acid for adjusting pH counted to 4, then in parts by weight, respectively weigh 55 parts of modifications
Cornstarch emulsion, 0.2 part of copper sulphate and 2 parts of composite oxidant are placed in three-necked flask, are stirred and are placed at 50 DEG C
Heating water bath 1h, obtains reaction solution and to 10% sodium sulfite solution of mass fraction of dropwise reaction liquid quality 2% in reaction solution, quiet
It sets and is cooled to room temperature, obtain mixed phase, filter to obtain filter residue, filter residue is washed with water 1 time, dried in 55 DEG C of baking ovens, crush, must aoxidize
Cornstarch takes oxidised maize starch and is mixed with deionized water, is configured to the corn starch milk of mass fraction 30%；By weight
Number meter, respectively weigh 45 parts 30% corn starch milk, 7 parts of sodium hydroxides, 0.2 part of tributyl phosphate, 0.1 part of second
Glycol, 0.6 part of polyvinyl alcohol（Mass fraction is 10%）, 0.3 part of ammonium persulfate, 12 parts of acrylamide and 5 parts of ethylene
30% corn starch milk is added in three isopropoxy silane of base in four-hole boiling flask, under 50 DEG C of water-baths, stirs 15min, heating
To 88 DEG C, sodium hydroxide is added, is gelatinized 25min, is subsequently cooled to 50 DEG C, tributyl phosphate, ethylene glycol and mass fraction is added
For 10% polyvinyl alcohol, after leading to nitrogen 6min, start that ammonium persulfate and acrylamide is added dropwise, control drips off in 3h, works as grafting
After reaction carries out 1.5h, start that vinyl silane triisopropoxide is added dropwise, control drips off in 1h, and graft copolymerization 4h is cooled to
Room temperature is up to corn starch adhesive；It counts in parts by weight, weighs 7 parts of Nano-meter SiO_2 respectively2, 45 parts by weight absolute ethyl alcohol/
Water（Volume ratio is 3 ︰ 1）, 2 parts of 0.2% silane coupling agent, by Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water,
Keep its fully dispersed under 4000r/min high speed shears, adjusts shear rate to 2000r/min, 70 DEG C or so of reaction temperature adds
The silane coupling agent for entering 0.2% is obtained suspension after reacting 95min, is filtered to obtain filter cake with oxalic acid solution regulation system pH value to 4,
Filter cake puts dry 1h under 80 DEG C of baking ovens, is cooled to room temperature and grinds to get modified Nano SiO2Powder；It counts in parts by weight, point
Also known as measure 4 parts of modified Nano SiO2Powder, 25 parts by weight Corn starch adhesive, by modified Nano at 50 DEG C of ultrasonic device
SiO2Powder is slowly added in corn starch adhesive, adds persistent oscillation 1h to get modified corn starch adhesive.
In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；It is 40% to prepare mass fraction
Cornstarch emulsion, with mass fraction be 3% salt acid for adjusting pH counted to 5, then in parts by weight, respectively weigh 60 parts of modifications
Cornstarch emulsion, 0.3 part of copper sulphate and 3 parts of composite oxidant are placed in three-necked flask, are stirred and are placed at 55 DEG C
Heating water bath 2h, obtains reaction solution and to 10% sodium sulfite solution of mass fraction of dropwise reaction liquid quality 2% in reaction solution, quiet
It sets and is cooled to room temperature, obtain mixed phase, filter to obtain filter residue, filter residue is washed with water 2 times, dried in 60 DEG C of baking ovens, crush, must aoxidize
Cornstarch takes oxidised maize starch and is mixed with deionized water, is configured to the corn starch milk of mass fraction 30%；By weight
Number meter, respectively weigh 50 parts 30% corn starch milk, 8 parts of sodium hydroxides, 0.3 part of tributyl phosphate, 0.2 part of second
Glycol, 0.7 part of polyvinyl alcohol（Mass fraction is 10%）, 0.4 part of ammonium persulfate, 14 parts of acrylamide and 6 parts of ethylene
30% corn starch milk is added in three isopropoxy silane of base in four-hole boiling flask, under 55 DEG C of water-baths, stirs 20min, heating
To 90 DEG C, sodium hydroxide is added, is gelatinized 30min, is subsequently cooled to 55 DEG C, tributyl phosphate, ethylene glycol and mass fraction is added
For 10% polyvinyl alcohol, after leading to nitrogen 8min, start that ammonium persulfate and acrylamide is added dropwise, control drips off in 4h, works as grafting
After reaction carries out 2h, start that vinyl silane triisopropoxide is added dropwise, control drips off in 2h, and graft copolymerization 5h is cooled to room
Temperature is up to corn starch adhesive；It counts in parts by weight, weighs 8 parts of Nano-meter SiO_2 respectively2, 50 parts by weight absolute ethyl alcohol/water
（Volume ratio is 3 ︰ 1）, 3 parts of 0.3% silane coupling agent, by Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water,
Keep its fully dispersed under 4000r/min high speed shears, adjusts shear rate to 2000r/min, 75 DEG C or so of reaction temperature is added
0.3% silane coupling agent is obtained suspension after reacting 100min, filters to obtain filter cake, filtered with oxalic acid solution regulation system pH value to 5
Cake puts dry 2h under 80 DEG C of baking ovens, is cooled to room temperature and grinds to get modified Nano SiO2Powder；It counts in parts by weight, respectively
Weigh 5 parts of modified Nano SiO2Powder, 30 parts by weight Corn starch adhesive, by modified Nano at 55 DEG C of ultrasonic device
SiO2Powder is slowly added in corn starch adhesive, adds persistent oscillation 2h to get modified corn starch adhesive.
Reference examples：The starch adhesive of Jiangxi company production
The adhesive of example and reference examples is detected, specific detection is as follows：
Drying time：Adhesive is coated on label paper, vial is affixed on, weighs on assay balance at once, weight includes
The quality sum of moisture and solid four in bottle, trade mark, adhesive（W1）.Drying at room temperature after having claimed, weighs every 2h
Once, you can obtain the corresponding quality of 2h, 4h, 6h, 8h（W2, W3, W4, W5 etc.）.Later, sample is placed in drier
2 days, so that sample is completely dried and be re-weighed once.This inferior quality is considered bottle, trade mark and three quality sums with solid
（WH）.Aqueous quality is set as W in adhesive, then W=W1-WH, and the biodiversity lost within 2h is W1-W2.Thus it counts
Calculate the ratio that moisture content is lost in 2h：Fluid loss=（W1-W2）/ W uses same method, can obtain the mistake of 4h, 6h, 8h
Water ratio.Using the time as horizontal axis, dehydration ratio is the longitudinal axis, obtains the drying curve of adhesive.Dehydration is found out on drying curve
Time used when 80%, the drying time as the sample.
Adhesion strength is tested：Under constant temperature and humidity, dacron membrane is cut into 16cm × 1.5cm strips, by a certain amount of gluing
Agent is applied to the one side of dacron membrane item, another is sticked on one of gluing, cohesive length is fixed as 10cm.By what is bonded
After waiting adhesive surfaces to be completely dried, pulling force is tested using CSS-44010 almighty test machines for paper slip drying at room temperature.It tests parallel
Style 5, load results take the average value of 5 tests.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Drying time/h | 0.5 | 0.3 | 0.7 | 5.0 |
| Adhesion strength/Pa.s | 56.0 | 54.6 | 52.3 | 31.0 |
As shown in Table 1, the starch adhesive that prepared by the present invention has drying time fast, the high advantage of adhesion strength.
Claims (1)
1. a kind of preparation method of modified corn starch adhesive, it is characterised in that specifically preparation process is：
（1）In mass ratio 4：1 weighs hydrogen peroxide and potassium peroxydisulfate mixing, obtains composite oxidant；
（2）The cornstarch emulsion that mass fraction is 40% is prepared, the salt acid for adjusting pH for being 3% with mass fraction is to 3~5, then presses
Parts by weight meter weighs 50~60 parts of modified corn starch lotions, 0.1~0.3 part of copper sulphate and 1~3 part of composite oxygen respectively
Agent is placed in three-necked flask, is stirred and is placed in 1~2h of heating water bath at 45~55 DEG C, obtains reaction solution and in reaction solution
10% sodium sulfite solution of mass fraction of dropwise reaction liquid quality 2%, standing are cooled to room temperature, and obtain mixed phase, filter to obtain filter
Slag, is washed with water filter residue 1~2 time, is dried in 50~60 DEG C of baking ovens, crushes, obtains oxidised maize starch, take oxidised maize starch
And mixed with deionized water, it is configured to the corn starch milk of mass fraction 30%；
（3）It counts in parts by weight, respectively 30% corn starch milk of 40~50 parts of weighing, 6~8 parts of sodium hydroxides, 0.1~0.3
The tributyl phosphate, 0.1~0.2 part of ethylene glycol, 0.5~0.7 part of polyvinyl alcohol of part（Mass fraction is 10%）, 0.2~
0.4 part of ammonium persulfate, 10~14 parts of acrylamide and 5~6 parts of vinyl silane triisopropoxide, in four-hole boiling flask
30% corn starch milk is added, under 45~55 DEG C of water-baths, stirs 10~20min, is warming up to 85~90 DEG C, hydroxide is added
Sodium is gelatinized 20~30min, is subsequently cooled to 45~55 DEG C, be added tributyl phosphate, ethylene glycol and mass fraction be 10% it is poly-
Vinyl alcohol after leading to 4~8min of nitrogen, starts that ammonium persulfate and acrylamide is added dropwise, and control drips off in 3~4h, when grafting is anti-
After should carrying out 1.5~2h, starting that vinyl silane triisopropoxide is added dropwise, control drips off in 1~2h, 4~5h of graft copolymerization,
It is cooled to room temperature up to corn starch adhesive；
（4）It counts in parts by weight, weighs 6~8 parts of Nano-meter SiO_2 respectively2, 40~50 parts of absolute ethyl alcohol/water（Volume ratio is 3 ︰
1）, 2~3 parts of 0.2%~0.3% silane coupling agent, by Nano-meter SiO_22It is added in the mixed solution of absolute ethyl alcohol/water,
Keep its fully dispersed under 4000r/min high speed shears, adjusting shear rate to 2000r/min, 65~75 DEG C or so of reaction temperature,
0.2%~0.3% silane coupling agent is added, with oxalic acid solution regulation system pH value to 3~5, must be hanged after reacting 90~100min
Supernatant liquid, filters to obtain filter cake, and filter cake puts dry 1~2h under 80 DEG C of baking ovens, is cooled to room temperature and grinds to get modified Nano SiO2Powder
Body；
（5）It counts in parts by weight, weighs 4~5 parts of modified Nano SiO respectively2Powder, 20~30 parts of corn starch adhesives,
By modified Nano SiO at 45~55 DEG C of ultrasonic device2Powder is slowly added in corn starch adhesive, add persistent oscillation 1~
2h is to get modified corn starch adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810567956.8A CN108659751A (en) | 2018-06-05 | 2018-06-05 | A kind of preparation method of modified corn starch adhesive |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400729A (en) * | 2018-12-03 | 2019-03-01 | 寿光金远东变性淀粉有限公司 | A method of oxidized starch is prepared using composite oxidant |
| CN109989292A (en) * | 2019-03-01 | 2019-07-09 | 徐扣华 | A kind of preparation method of starch base sticking agent |
| CN110128557A (en) * | 2019-05-15 | 2019-08-16 | 河南汇泉生物科技有限公司 | A kind of oxidized starch and preparation method thereof |
| CN110183974A (en) * | 2019-05-20 | 2019-08-30 | 陈光辉 | The anti-glutinous rice glue and preparation method thereof that warps of one kind |
| CN110743286A (en) * | 2019-11-04 | 2020-02-04 | 中国华电科工集团有限公司 | Chemical agglomeration liquid, device, preparation method and application |
| CN110903407A (en) * | 2019-12-22 | 2020-03-24 | 南通通地生物技术有限公司 | Oxidized starch and preparation method thereof |
| CN110964467A (en) * | 2019-12-24 | 2020-04-07 | 彭敏 | High-strength adhesive for corrugated board and preparation method thereof |
| CN111087946A (en) * | 2019-12-20 | 2020-05-01 | 株洲工大彩色印刷有限公司 | Fiber-reinforced starch adhesive and preparation method thereof |
| CN113088222A (en) * | 2021-04-30 | 2021-07-09 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN117887383A (en) * | 2024-03-18 | 2024-04-16 | 潍坊市农业科学院(山东省农业科学院潍坊市分院) | Preparation method and application of plant fixing adhesive |
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2018
- 2018-06-05 CN CN201810567956.8A patent/CN108659751A/en not_active Withdrawn
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400729A (en) * | 2018-12-03 | 2019-03-01 | 寿光金远东变性淀粉有限公司 | A method of oxidized starch is prepared using composite oxidant |
| CN109989292A (en) * | 2019-03-01 | 2019-07-09 | 徐扣华 | A kind of preparation method of starch base sticking agent |
| CN110128557A (en) * | 2019-05-15 | 2019-08-16 | 河南汇泉生物科技有限公司 | A kind of oxidized starch and preparation method thereof |
| CN110183974A (en) * | 2019-05-20 | 2019-08-30 | 陈光辉 | The anti-glutinous rice glue and preparation method thereof that warps of one kind |
| CN110743286B (en) * | 2019-11-04 | 2024-04-19 | 中国华电科工集团有限公司 | Chemical agglomeration liquid, device, preparation method and application |
| CN110743286A (en) * | 2019-11-04 | 2020-02-04 | 中国华电科工集团有限公司 | Chemical agglomeration liquid, device, preparation method and application |
| CN111087946A (en) * | 2019-12-20 | 2020-05-01 | 株洲工大彩色印刷有限公司 | Fiber-reinforced starch adhesive and preparation method thereof |
| CN110903407A (en) * | 2019-12-22 | 2020-03-24 | 南通通地生物技术有限公司 | Oxidized starch and preparation method thereof |
| CN110964467A (en) * | 2019-12-24 | 2020-04-07 | 彭敏 | High-strength adhesive for corrugated board and preparation method thereof |
| CN113088222B (en) * | 2021-04-30 | 2022-08-23 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN113088222A (en) * | 2021-04-30 | 2021-07-09 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN117887383A (en) * | 2024-03-18 | 2024-04-16 | 潍坊市农业科学院(山东省农业科学院潍坊市分院) | Preparation method and application of plant fixing adhesive |
| CN117887383B (en) * | 2024-03-18 | 2024-06-11 | 潍坊市农业科学院(山东省农业科学院潍坊市分院) | Preparation method and application of plant fixing adhesive |
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