CN108586867A - A kind of preparation method of modified starch base vinyon - Google Patents
A kind of preparation method of modified starch base vinyon Download PDFInfo
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
- C08B31/006—Crosslinking of derivatives of starch
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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
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a kind of preparation methods of modified starch base vinyon, belong to plastics preparing technical field.Polyethylene is modified first with antimony oxide and red phosphorus, during being decomposed when heated due to antimony oxide and red phosphorus, it is unaffected to polyethylene, the present invention carries out potato starch using epoxychloropropane and succinic anhydride dual modified, under the action of modified starch, base material is set to form the interface of some strength, again by the way that graft copolymerization occurs with the activity hydroxy in starch, oxidation and esterification chemical reaction, wherein potato starch itself has excellent biodegradable, and it is nontoxic, it is nonirritant, continue that TiO is obtained by the reaction in the mixings such as butyl titanate and carbon tetrachloride using sol-gal process2Catalytic powder, due to TiO2Catalytic powder generates electronics and hole under the excitation of ultraviolet light, has very strong redox ability, further increases the degradability of vinyon, be with a wide range of applications.
Description
Technical field
The invention discloses a kind of preparation methods of modified starch base vinyon, belong to plastics preparing technical field.
Background technology
Vinyon（Referred to as：PE）, it is one of five big synthetic resin, is production capacity maximum, import in China's synthetic resin
Measure most kinds.With corrosion resistance, electrical insulating property（Especially high-frequency insulation）It is excellent, it can be with chlorination, the spies such as radiation modification
Point.It is mainly used for the departments such as packaging, agricultural and traffic.
It is multiple that polyethylene is widely used in plastic package material, expanded material, braiding cloth material, cable covering material etc.
Aspect.But its oxygen index (OI) only has 18.5, belongs to combustible material, and which has limited their applications.In order to improve polythene material
Anti-flammability, traditionally general addition retardant synergists such as halogen containing flame-retardant and antimony oxide, this fire retardant burning
When can discharge a large amount of toxic hydrogen halides, smog is big, can cause greatly to damage to environment and personal safety.Therefore,
Magnesium hydroxide, aluminium hydroxide as have both filling, fire-retardant, smoke elimination function clean type inorganic combustion inhibitor be one up-and-coming
It substituting, hydroxide can release moisture in burning, when material meets fire burning, can absorb the heat that burning is released,
Water and oxide are generated, there is certain the process of carbonization to polymer, a protective layer is formed, plays fire retardation, inhibit simultaneously
The generation of material combustion and smog, and achieve the purpose that Halogen, nontoxic, low cigarette, especially magnesium hydroxide has as fire retardant
Higher decomposition temperature.Since magnesium hydrate halogen-free fire retardant only can reach fire-retardant when the amount of being filled with reaches 50% or more
The effect of polymer, this causes the mechanical property of polymer material, especially toughness and intensity to be greatly lowered.On the other hand,
Due to magnesium hydroxide surface hydrophilic oleophobic, polarity is big, causes it under the conditions of high filler loading capacity, it is difficult to be evenly dispersed into macromolecule
In matrix, to influence the processing performance and mechanical performance of polymer material.Therefore, it is necessary to add a small amount of retardant synergist to drop
Low hydrogen magnesia dosage, to improve material property.
With the development of social economy and the progress of science and technology, the consciousness of people's environmental protection is higher and higher, plastics
White pollution problems caused by waste are also increasingly taken seriously, therefore, when the material with biodegradability becomes
The needs of generation development.However the degradability of current vinyon is poor, cannot meet the requirement to polyethylene of people, and resistance to
Aqueous difference.Therefore, a kind of good flame resistance, the modified starch base vinyon with degradability and water-tolerant are invented to plastics
Preparing technical field has positive effect.
Invention content
The technical problems to be solved by the invention：For current common PE plastics, there are poor fire, degradability are poor
And poor water resistance, it can not meet the defect of material market requirement, provide a kind of preparation side of modified starch base vinyon
Method.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of modified starch base vinyon, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, are mixed at being 80~85 DEG C in temperature
16~18min of stirring is closed, gelatinized corn starch liquid is obtained, naturally cools to 24~32 DEG C, the hydrochloric acid that mass fraction is 11% is used in combination to adjust
The pH value of gelatinized corn starch liquid obtains starch mixed liquor, then the different of starch mixed liquor quality 1% is added into starch mixed liquor to 5~6
Amylase, at being 32~35 DEG C in temperature after 47~52min of stirring enzymolysis, filtering removal filter residue, it is that starch is anti-to obtain filtrate
Answer liquid；
（2）Then starch reaction liquid, sodium hydroxide solution, epoxychloropropane and the succinic anhydride that mass fraction is 3% are pressed into matter
Amount is than being 5：1：2：1 mixing, and it is stirred to react 21~24min at being 35~40 DEG C in temperature, mixed liquor is obtained, continues to mix
Liquid is put into nutsch filter and filters 3~5 times, and removal filtrate obtains modified starch to get solids, natural air drying, grinding discharging
Grain；
（3）It weighs 5~7mL butyl titanates to pour into the beaker with 16~20mL carbon tetrachloride, and is mixed, mixed
Liquid is closed, then 2~4mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reaction after hydrolysis, obtains g., jelly-like colloidal sol, continues
G., jelly-like colloidal sol is placed in cucurbit and is distilled, fluffy powder is obtained, fluffy powder is finally poured into Muffle kiln roasting, is ground
Discharging, obtains TiO2Catalytic powder；
（4）Weighing 68~76g polyethylene heat temperature raisings makes its softening, and 1~3g, tri- oxygen is sequentially added into the polyethylene after softening
Change two antimony and 2~4g red phosphorus, continue to be mixed, obtains modified poly ethylene molten liquid；
（5）It counts in parts by weight, weighs 35~40 parts of modified poly ethylene molten liquids, 13~15 parts of modified starch particles and 9 respectively
~11 parts of TiO2Catalytic powder mixing, which is placed in reaction kettle, to be stirred to react, then adds 2~4 parts of stearic acid, 1~3 part of benzoyl peroxide
Formyl and 3~5 parts of absolute ethyl alcohols continue heat preservation and are mixed, obtain mixture, continue mixture being put into double screw extruder
Middle mixing is granulated, and extrusion molding is to get modified starch base vinyon.
Step（1）The mass ratio of the potato starch and deionized water is 1：7, whipping temp is 80~85 DEG C, is stirred
It is 16~18min to mix the time, and cooling temperature is 24~32 DEG C, and the mass fraction of hydrochloric acid is 11%, stirring hydrolysis temperature is 32~
35 DEG C, stirring enzymolysis time is 47~52min.
Step（2）The starch reaction liquid, sodium hydroxide solution, epoxychloropropane and the amber that mass fraction is 3%
The mass ratio of acid anhydrides is 5：1：2：1, it is 35~40 DEG C to be stirred to react temperature, and it is 21~24min to be stirred to react the time, filters number
It is 3~5 times.
Step（3）The mixing time be 6~9min, hydrolysis time be 35~40min, vapo(u)rizing temperature be 45~
50 DEG C, distillation time is 45~60min, and calcination temperature is 550~600 DEG C, and roasting time is 1~2h.
Step（4）The heat temperature raising temperature is 85~90 DEG C, and mixing time is 30~32min.
Step（5）The temperature that is stirred to react is 120~125 DEG C, and it is 45~60min to be stirred to react the time, continues to stir
It is 17~19min to mix the time, and melting temperature is 160~240 DEG C, and mixing pressure is 2~4MPa, and mixing time is 1~2h.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is using polyethylene as base material, modified starch particle and TiO2Catalytic powder is aided with stearic acid as accelerating agent
Modified starch base vinyon is prepared with benzoyl peroxide etc., first with antimony oxide and red phosphorus to polyethylene
It is modified, during being decomposed when heated due to antimony oxide and red phosphorus, unaffected to polyethylene, these are fire-retardant
Agent is crosslinked with polyethylene reacts, and generates layer of charcoal or foam-like covering, blocks air contact polyethylene surface, control
Volatilizable fuel enters air accelerated combustion, realizes the effect for slowing down heat and mass, to improve vinyon
Anti-flammability；
（2）The present invention is dual modified to potato starch progress using epoxychloropropane and succinic anhydride, in the work of modified starch
Under, base material is made to form the interface of some strength, esterification can replace by hydroxyl and assign starch hydrophobicity, and crosslinking Treatment increases
Add intramolecule and intermolecular contact, while crosslinked density in starch structure can be increased, to limit the absorption of moisture,
So that the starch with certain viscosity is dispersed in polyethylene surface, enhancing starch and polyolefins compatibility, then by with
Graft copolymerization, oxidation and esterification chemical reaction occur for the activity hydroxy in starch, promote the content for reducing surface hydroxyl, reach thin
The purpose of water, to improve the water resistance of vinyon, wherein potato starch itself has excellent biodegradable,
And it is nontoxic, nonirritant, the effects that its microorganism in nature, water, acid, alkali under can decompose completely, final product is
Carbon dioxide and water, it is environmentally safe, to improve the degradability of vinyon, continue to use sol-gel method will
TiO is obtained by the reaction in the mixings such as butyl titanate and carbon tetrachloride2Catalytic powder, due to TiO2Catalytic powder is in ultraviolet light
Excitation is lower to generate electronics and hole, has very strong redox ability, it is thorough will to be adsorbed on surrounding macromolecule organic
Bottom is oxidized to carbon dioxide and water, further increases the degradability of vinyon, is with a wide range of applications.
Specific implementation mode
It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, in the case where temperature is 80~85 DEG C
16~18min is mixed, obtains gelatinized corn starch liquid, naturally cools to 24~32 DEG C, it is 11% hydrochloric acid tune that mass fraction, which is used in combination,
The pH value of gelatinized corn starch liquid is saved to 5~6, obtains starch mixed liquor, then starch mixed liquor quality 1% is added into starch mixed liquor
Isoamylase, at being 32~35 DEG C in temperature after 47~52min of stirring enzymolysis, filtering removal filter residue, it is starch to obtain filtrate
Reaction solution；Then starch reaction liquid, sodium hydroxide solution, epoxychloropropane and the succinic anhydride that mass fraction is 3% are pressed into matter
Amount is than being 5：1：2：1 mixing, and it is stirred to react 21~24min at being 35~40 DEG C in temperature, mixed liquor is obtained, continues to mix
Liquid is put into nutsch filter and filters 3~5 times, and removal filtrate obtains modified starch to get solids, natural air drying, grinding discharging
Grain；It weighs 5~7mL butyl titanates to pour into the beaker with 16~20mL carbon tetrachloride, and 6~9min is mixed, obtain
To mixed liquor, then 2~4mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reacts 35~40min, after hydrolysis, obtains fruit
Freeze shape colloidal sol, continue g., jelly-like colloidal sol being placed in cucurbit, distills 45~60min at being 45~50 DEG C in temperature, obtain fluffy
Loose powder end, finally pours into fluffy powder in Muffle furnace, and 1~2h is roasted under conditions of temperature is 550~600 DEG C, is ground
Material, obtains TiO2Catalytic powder；Weighing 68~76g polyethylene and being heated to 85~90 DEG C makes its softening, to poly- after softening
1~3g antimony oxides and 2~4g red phosphorus are sequentially added in ethylene, are continued 30~32min of mixing, are obtained modified poly ethylene
Molten liquid；It counts in parts by weight, weighs 35~40 parts of modified poly ethylene molten liquids, 13~15 parts of modified starch particles and 9 respectively
~11 parts of TiO2Catalytic powder mixing is placed in reaction kettle, is stirred to react 45~60min at being 120~125 DEG C in temperature, then add
Add 2~4 parts of stearic acid, 1~3 part of benzoyl peroxide and 3~5 parts of absolute ethyl alcohols, continue heat preservation and 17~19min is mixed,
Mixture is obtained, continues mixture being put into double screw extruder, temperature is 160~240 DEG C, pressure is 2~4MPa's
Under the conditions of be kneaded 1~2h, be granulated, extrusion molding is to get modified starch base vinyon.
Example 1
It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, are mixed at being 80 DEG C in temperature
16min obtains gelatinized corn starch liquid, naturally cools to 24 DEG C, and the hydrochloric acid that mass fraction is 11% is used in combination to adjust the pH value of gelatinized corn starch liquid
To 5, starch mixed liquor is obtained, then the isoamylase of starch mixed liquor quality 1% is added into starch mixed liquor, is 32 in temperature
At DEG C after stirring enzymolysis 47min, filtering removal filter residue, it is starch reaction liquid to obtain filtrate；Then by starch reaction liquid, quality
Sodium hydroxide solution, epoxychloropropane and the succinic anhydride that score is 3% are 5 in mass ratio：1：2：1 mixing, and be in temperature
It is stirred to react 21min at 35 DEG C, obtains mixed liquor, continues mixed liquor being put into nutsch filter suction filtration 3 times, removal filtrate is to get solid
Body object, natural air drying, grinding discharging obtain modified starch particle；5mL butyl titanates are weighed to pour into 16mL carbon tetrachloride
Beaker in, and 6min is mixed, obtains mixed liquor, then 2mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reaction
35min after hydrolysis, obtains g., jelly-like colloidal sol, continues g., jelly-like colloidal sol being placed in cucurbit, is steamed at being 45 DEG C in temperature
45min is evaporated, fluffy powder is obtained, finally pours into fluffy powder in Muffle furnace, 1h is roasted under conditions of temperature is 550 DEG C,
Grinding discharging, obtains TiO2Catalytic powder；Weighing 68g polyethylene and being heated to 85 DEG C makes its softening, to the poly- second after softening
1g antimony oxides and 2g red phosphorus are sequentially added in alkene, are continued that 30min is mixed, are obtained modified poly ethylene molten liquid；By weight
Number meter is measured, weighs 35 parts of modified poly ethylene molten liquids, 13 parts of modified starch particles and 9 parts of TiO respectively2Catalytic powder mixing is set
In reaction kettle, it is stirred to react 45min at being 120 DEG C in temperature, then add 2 parts of stearic acid, 1 part of benzoyl peroxide and 3 parts
Absolute ethyl alcohol continues heat preservation and 17min is mixed, obtains mixture, continue mixture being put into double screw extruder, in temperature
Degree is 160 DEG C, pressure is kneaded 1h under conditions of being 2MPa, is granulated, extrusion molding is to get modified starch base vinyon.
Example 2
It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, are mixed at being 82 DEG C in temperature
17min obtains gelatinized corn starch liquid, naturally cools to 28 DEG C, and the hydrochloric acid that mass fraction is 11% is used in combination to adjust the pH value of gelatinized corn starch liquid
To 5, starch mixed liquor is obtained, then the isoamylase of starch mixed liquor quality 1% is added into starch mixed liquor, is 34 in temperature
At DEG C after stirring enzymolysis 49min, filtering removal filter residue, it is starch reaction liquid to obtain filtrate；Then by starch reaction liquid, quality
Sodium hydroxide solution, epoxychloropropane and the succinic anhydride that score is 3% are 5 in mass ratio：1：2：1 mixing, and be in temperature
It is stirred to react 22min at 37 DEG C, obtains mixed liquor, continues mixed liquor being put into nutsch filter suction filtration 4 times, removal filtrate is to get solid
Body object, natural air drying, grinding discharging obtain modified starch particle；6mL butyl titanates are weighed to pour into 18mL carbon tetrachloride
Beaker in, and 7min is mixed, obtains mixed liquor, then 3mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reaction
37min after hydrolysis, obtains g., jelly-like colloidal sol, continues g., jelly-like colloidal sol being placed in cucurbit, is steamed at being 47 DEG C in temperature
47min is evaporated, fluffy powder is obtained, finally pours into fluffy powder in Muffle furnace, is roasted under conditions of temperature is 570 DEG C
1.5h, grinding discharging, obtains TiO2Catalytic powder；Weighing 72g polyethylene and being heated to 87 DEG C makes its softening, to after softening
2g antimony oxides and 3g red phosphorus are sequentially added in polyethylene, are continued that 31min is mixed, are obtained modified poly ethylene molten liquid；
It counts in parts by weight, weighs 37 parts of modified poly ethylene molten liquids, 14 parts of modified starch particles and 10 parts of TiO respectively2Catalytic powder
Mixing is placed in reaction kettle, is stirred to react 55min at being 122 DEG C in temperature, then add 3 parts of stearic acid, 2 parts of benzoyl peroxides
With 4 parts of absolute ethyl alcohols, continues heat preservation and 18min is mixed, obtain mixture, continue mixture being put into double screw extruder
In, it is kneaded 1.5h under conditions of temperature is 200 DEG C, pressure is 3MPa, is granulated, extrusion molding is to get the poly- second of modified starch base
Alkene plastics.
Example 3
It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, are mixed at being 85 DEG C in temperature
18min obtains gelatinized corn starch liquid, naturally cools to 32 DEG C, and the hydrochloric acid that mass fraction is 11% is used in combination to adjust the pH value of gelatinized corn starch liquid
To 6, starch mixed liquor is obtained, then the isoamylase of starch mixed liquor quality 1% is added into starch mixed liquor, is 35 in temperature
At DEG C after stirring enzymolysis 52min, filtering removal filter residue, it is starch reaction liquid to obtain filtrate；Then by starch reaction liquid, quality
Sodium hydroxide solution, epoxychloropropane and the succinic anhydride that score is 3% are 5 in mass ratio：1：2：1 mixing, and be in temperature
It is stirred to react 24min at 40 DEG C, obtains mixed liquor, continues mixed liquor being put into nutsch filter suction filtration 5 times, removal filtrate is to get solid
Body object, natural air drying, grinding discharging obtain modified starch particle；7mL butyl titanates are weighed to pour into 20mL carbon tetrachloride
Beaker in, and 9min is mixed, obtains mixed liquor, then 4mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reaction
40min after hydrolysis, obtains g., jelly-like colloidal sol, continues g., jelly-like colloidal sol being placed in cucurbit, is steamed at being 50 DEG C in temperature
60min is evaporated, fluffy powder is obtained, finally pours into fluffy powder in Muffle furnace, 2h is roasted under conditions of temperature is 600 DEG C,
Grinding discharging, obtains TiO2Catalytic powder；Weighing 76g polyethylene and being heated to 90 DEG C makes its softening, to the poly- second after softening
3g antimony oxides and 4g red phosphorus are sequentially added in alkene, are continued that 32min is mixed, are obtained modified poly ethylene molten liquid；By weight
Number meter is measured, weighs 40 parts of modified poly ethylene molten liquids, 15 parts of modified starch particles and 11 parts of TiO respectively2Catalytic powder mixes
It is placed in reaction kettle, is stirred to react 60min at being 125 DEG C in temperature, then add 4 parts of stearic acid, 3 parts of benzoyl peroxides and 5
Part absolute ethyl alcohol continues heat preservation and 19min is mixed, obtains mixture, continue mixture being put into double screw extruder,
Temperature is 240 DEG C, pressure is kneaded 2h under conditions of being 4MPa, is granulated, extrusion molding is to get modified starch base vinyon.
Comparative example
With the modified starch base vinyon of Guangdong company production as a comparison case to modified starch base produced by the present invention
Modified starch base vinyon in vinyon and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Degradation rate test is detected by GB/T19277 standards after 90 days；
Flame retardant rating test is by flame retardant rating by HB, and incremental standard is detected step by step to V-0 by V-2, V-1；
Oxygen index (OI) test carries out performance detection using oxygen index measurer；
Horizontal firing length testing is detected by GB/T2408 combustibility test method horizontal firing methods；
Vertical combustion time test measures normal beam technique by GB/T5455 flame retardant properties and is detected；
Water absorption rate test is detected by GB T 3299-2011 standards；
Water resistance test：Vinyon in example 1~3 and comparative example is placed in wet condition, each polyethylene is measured
The tensile strength and fracture strength of plastics.
1 vinyon performance measurement result of table
According to the modified starch base vinyon good flame resistance produced by the present invention of data among the above, flame retardant rating reaches 0
Grade, degradation rate is high, and degradation rate reaches 97% after 90 days, and water-tolerant, water absorption rate is low, in wet condition, tensile strength and fracture
Intensity is high, has broad application prospects.
Claims (6)
1. a kind of preparation method of modified starch base vinyon, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio：7 are placed in potato starch and deionized water mixing in beaker, are mixed at being 80~85 DEG C in temperature
16~18min of stirring is closed, gelatinized corn starch liquid is obtained, naturally cools to 24~32 DEG C, the hydrochloric acid that mass fraction is 11% is used in combination to adjust
The pH value of gelatinized corn starch liquid obtains starch mixed liquor, then the different of starch mixed liquor quality 1% is added into starch mixed liquor to 5~6
Amylase, at being 32~35 DEG C in temperature after 47~52min of stirring enzymolysis, filtering removal filter residue, it is that starch is anti-to obtain filtrate
Answer liquid；
（2）Then starch reaction liquid, sodium hydroxide solution, epoxychloropropane and the succinic anhydride that mass fraction is 3% are pressed into matter
Amount is than being 5：1：2：1 mixing, and it is stirred to react 21~24min at being 35~40 DEG C in temperature, mixed liquor is obtained, continues to mix
Liquid is put into nutsch filter and filters 3~5 times, and removal filtrate obtains modified starch to get solids, natural air drying, grinding discharging
Grain；
（3）It weighs 5~7mL butyl titanates to pour into the beaker with 16~20mL carbon tetrachloride, and is mixed, mixed
Liquid is closed, then 2~4mL distilled water is added dropwise into mixed liquor, mixed hydrolysis reaction after hydrolysis, obtains g., jelly-like colloidal sol, continues
G., jelly-like colloidal sol is placed in cucurbit and is distilled, fluffy powder is obtained, fluffy powder is finally poured into Muffle kiln roasting, is ground
Discharging, obtains TiO2Catalytic powder；
（4）Weighing 68~76g polyethylene heat temperature raisings makes its softening, and 1~3g, tri- oxygen is sequentially added into the polyethylene after softening
Change two antimony and 2~4g red phosphorus, continue to be mixed, obtains modified poly ethylene molten liquid；
（5）It counts in parts by weight, weighs 35~40 parts of modified poly ethylene molten liquids, 13~15 parts of modified starch particles and 9 respectively
~11 parts of TiO2Catalytic powder mixing, which is placed in reaction kettle, to be stirred to react, then adds 2~4 parts of stearic acid, 1~3 part of benzoyl peroxide
Formyl and 3~5 parts of absolute ethyl alcohols continue heat preservation and are mixed, obtain mixture, continue mixture being put into double screw extruder
Middle mixing is granulated, and extrusion molding is to get modified starch base vinyon.
2. a kind of preparation method of modified starch base vinyon according to claim 1, it is characterised in that：Step
（1）The mass ratio of the potato starch and deionized water is 1：7, whipping temp be 80~85 DEG C, mixing time be 16~
18min, cooling temperature are 24~32 DEG C, and the mass fraction of hydrochloric acid is 11%, and stirring hydrolysis temperature is 32~35 DEG C, stirring enzymolysis
Time is 47~52min.
3. a kind of preparation method of modified starch base vinyon according to claim 1, it is characterised in that：Step
（2）The mass ratio of the starch reaction liquid, the sodium hydroxide solution that mass fraction is 3%, epoxychloropropane and succinic anhydride
It is 5：1：2：1, it is 35~40 DEG C to be stirred to react temperature, and it is 21~24min to be stirred to react the time, and it is 3~5 times to filter number.
4. a kind of preparation method of modified starch base vinyon according to claim 1, it is characterised in that：Step
（3）The mixing time is 6~9min, and hydrolysis time is 35~40min, and vapo(u)rizing temperature is 45~50 DEG C, when distillation
Between be 45~60min, calcination temperature be 550~600 DEG C, roasting time be 1~2h.
5. a kind of preparation method of modified starch base vinyon according to claim 1, it is characterised in that：Step
（4）The heat temperature raising temperature is 85~90 DEG C, and mixing time is 30~32min.
6. a kind of preparation method of modified starch base vinyon according to claim 1, it is characterised in that：Step
（5）The described temperature that is stirred to react is 120~125 DEG C, and it is 45~60min to be stirred to react the time, continue mixing time be 17~
19min, melting temperature are 160~240 DEG C, and mixing pressure is 2~4MPa, and mixing time is 1~2h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810355130.5A CN108586867A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of modified starch base vinyon |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810355130.5A CN108586867A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of modified starch base vinyon |
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| CN201810355130.5A Withdrawn CN108586867A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of modified starch base vinyon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015125A (en) * | 2021-10-20 | 2022-02-08 | 界首市天鸿新材料股份有限公司 | Preparation method of antistatic biodegradable packaging film |
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| CN1239725A (en) * | 1999-06-22 | 1999-12-29 | 沈阳南阳经贸集团有限公司 | Polynary degradable resin composition and its preparation process |
| CN101993558A (en) * | 2009-08-09 | 2011-03-30 | 陈天云 | Thin film produced by using starch fiber waste plastic |
| US20170183422A1 (en) * | 2015-08-04 | 2017-06-29 | Jiangnan University | Fluorescent Starch Nanocrystal and Preparation Method and Application thereof |
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| CN1239725A (en) * | 1999-06-22 | 1999-12-29 | 沈阳南阳经贸集团有限公司 | Polynary degradable resin composition and its preparation process |
| CN101993558A (en) * | 2009-08-09 | 2011-03-30 | 陈天云 | Thin film produced by using starch fiber waste plastic |
| US20170183422A1 (en) * | 2015-08-04 | 2017-06-29 | Jiangnan University | Fluorescent Starch Nanocrystal and Preparation Method and Application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015125A (en) * | 2021-10-20 | 2022-02-08 | 界首市天鸿新材料股份有限公司 | Preparation method of antistatic biodegradable packaging film |
| CN114015125B (en) * | 2021-10-20 | 2022-09-09 | 界首市天鸿新材料股份有限公司 | Preparation method of antistatic biodegradable packaging film |
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Application publication date: 20180928 |