CN108504285A - A kind of preparation method of food packaging fire-retardant bubble chamber film - Google Patents
A kind of preparation method of food packaging fire-retardant bubble chamber film Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D189/00—Coating compositions based on proteins; Coating compositions based on derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/675—Low-molecular-weight compounds
- C08G18/6765—Low-molecular-weight compounds containing the unsaturation at least partially in a cyclic ring having at least one oxygen atom in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The present invention relates to field of polymer material preparing technology, and in particular to a kind of preparation method of food packaging fire-retardant bubble chamber film.The present invention is under conditions of sodium methoxide and catalyst compounded triethanolamine by epoxidized soybean oil catalyzed alcoholysis,Obtain alcoholysis soybean oil,Hexamethylene diisocyanate is added,The raw materials such as diethyl phosphate,Obtain polyurethane foam,Methyltriethoxysilane is added in alkalizing flame-proof material to self-control,Obtain Silica hydrogel microencapsulation ammonium polyphosphate,Again fire retardant adhesive is obtained with soybean albumen adhesive mixed preparing,The single side that fire retardant adhesive is coated on to PVC film obtains composite membrane,It is finally putting into hot pressing in hot press and obtains food packaging fire-retardant bubble chamber film,Soybean albumen adhesive can be crosslinked with polyurethane foam and be reacted in the present invention,Cementation between polyurethane foam and PVC film is set to enhance,The mixed catalyst of sodium methoxide and triethanolamine has good dissolubility in the reaction system,The conversion ratio of ester exchange reaction can be improved,It is with a wide range of applications.
Description
Technical field
The present invention relates to field of polymer material preparing technology, and in particular to a kind of system of food packaging fire-retardant bubble chamber film
Preparation Method.
Background technology
Bubble chamber film is also known as air-cushion film, gas pearl film, bubble cloth, bubble paper, bubble film, bubble film, air bubble film.It is with height
Pressure polyethylene is primary raw material, then adds the auxiliary materials such as brightening agent, opening agent, and plastic uptake is squeezed out into bubble through 230 DEG C or so high temperature
Product.It is the New Plastic Packing Materials that a kind of quality is light, the transparency is good, nontoxic, tasteless, has good damping property, resists
Impact, heat sealer, it is nontoxic, tasteless, moisture-proof, corrosion-resistant, transparency is good the advantages that, be widely used in electronics, instrument, ceramics,
The fields such as craftwork, household electrical appliance, furniture and paint product product, glassware.
China market greatly increases the demand of this based packaging material, environmental protection is wanted with the fast development of electric business
Ask higher and higher, product characteristic is more and more prominent, and production cost is in rising trend always, also there are a large amount of enterprises using again on the market
Raw material recycle, but product quality can not ensure, workpiece surface easy to wear, especially lacquer painting, and intensity is not very
Height, noxious material can not avoid, and transparency is inadequate, the indexs all effected such as tensile strength.
As the improvement of people's living standards, people gradually recognize the importance of environmental protection.Currently, bubble chamber film in the market
Quality is bad, cracky, and most antistatic property, poor fire, degradability are poor, mechanical property is poor, they when discarded,
Environment easy to pollute, and it is difficult to recycling, the carcinogens such as bioxin can be formed when burning, and serious dirt is generated to air
Dye, endangers the health of people.In today of petroleum resources increasingly depleted and " white pollution " getting worse, conventional petroleum base
Packaging material certainly will not be the trend place of future development, and environmental-friendly degradable package material will be that solution petroleum resources are withered
It exhausts and the preferred material of " white pollution ".
Therefore, a kind of bubble chamber film that can solve above-mentioned performance issue is developed to have important practical significance.
Invention content
Present invention mainly solves the technical issues of, for bubble chamber film poor flame retardant properties currently on the market, when bubble chamber film is used
When food and Key works Drug packing, since existing bubble chamber film is often using PVC film as film layer material, and active chlorine is former in PVC film
Son is unstable, is easy to decomposite toxic substance, influences the defect of health, provides a kind of food packaging fire-retardant bubble
The preparation method of film.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of food packaging fire-retardant bubble chamber film, it is characterised in that specifically preparation process is：
（1）200~220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, uses sodium hydroxide solution
PH is adjusted, to four-hole boiling flask heat temperature raising, is added 60~70g soy meals, after isothermal holding, it is added 10 into four-hole boiling flask~
12g phenol, cooling, isothermal holding continue that 20~25mL formaldehyde is added into four-hole boiling flask, and reaction, cooled to room temperature obtains
To soybean albumen adhesive；
（2）70~80mL epoxidized soybean oils, 4~5g methanol are added into the three-necked flask with dropping funel and condensing unit
Sodium, 5~7mL triethanolamines, heat temperature raising are started blender and are stirred with the rotating speed of 200~300r/min, to three-necked flask
Middle addition 40~50mL glycerine, insulated and stirred reaction, obtains alcoholysis soybean oil；
（3）80~90mL hexamethylene diisocyanates are added into above-mentioned three-necked flask, the reaction was continued for 8~10mL styrene, waits for three mouthfuls
Flask cools down, and 10~15mL diethyl phosphates, 20~30mL glycerine and 20~25mL maleic acids is added into three-necked flask successively
Acid anhydride pours into after separately taking 3~5mL dibutyl tin laurates to be dissolved in 35~40mL acetone in constant pressure funnel, then instills three mouthfuls
In flask, heat up when being added dropwise, the reaction was continued, obtains polyurethane foam；
（4）100~120g ammonium polyphosphate, 230~250mL absolute ethyl alcohols, 100~120mL distilled water, stirring are added into beaker
Ammonium hydroxide adjusting pH is added into beaker, obtains alkalization flame-proof material for mixing；
（5）20~25g methyltriethoxysilane is added into alkalization flame-proof material, to beaker water-bath heat temperature raising, insulation reaction,
Filtering removal filtrate, obtains gel, after gel is washed with distilled water 2~3 times, is put into baking oven, heat temperature raising, dry, obtains
To Silica hydrogel microencapsulation ammonium polyphosphate；
（6）Soybean albumen adhesive and Silica hydrogel microencapsulation ammonium polyphosphate are mixed to get fire retardant adhesive, by retardant adhesive
Agent is coated on the single side of PVC film, and polyurethane foam is put into formalin and is impregnated, and being put into two panels as interlayer after taking-up applies
It is furnished between the PVC film of fire retardant adhesive, obtains composite membrane, composite membrane is put into hot pressing in hot press, obtains food packaging
With fire-retardant bubble chamber film.
Step（1）The mass fraction of the sodium hydroxide solution is 40%, and it is 9~10 to adjust pH with sodium hydroxide solution,
It it is 90~100 DEG C to temperature after four-hole boiling flask heat temperature raising, the isothermal holding time is 50~55min, temperature after cooling after heating
It it is 70~75 DEG C, the isothermal holding time is 15~20min after cooling, and the reaction time is 1~2h.
Step（2）Temperature is 50~60 DEG C after the heat temperature raising, and agitator speed is 200~300r/min, heat preservation
It is 3~4h to be stirred to react the time.
Step（3）The styrene the reaction was continued time is 2~3h, and temperature is 50~60 DEG C after three-necked flask cooling,
Constant pressure funnel drop rate is 2~3mL/min, and control heating rate is 3~5 DEG C/min, and temperature is 80~82 after heating
DEG C, the reaction was continued, and the time is 3~4h.
Step（4）Described to be stirred the time as 20~25min, the mass fraction of ammonium hydroxide is 35%, and ammonia is added into beaker
It is 10.2~10.4 that water, which adjusts pH,.
Step（5）Described is 45~60 DEG C to temperature after beaker water-bath heat temperature raising, and the insulation reaction time is 2~3h,
Temperature is 80~90 DEG C after baking oven heat temperature raising, and drying time is 5~6h.
Step（6）The soybean albumen adhesive is 5 ︰ 1 with Silica hydrogel microencapsulation ammonium polyphosphate mixing quality ratio,
PVC film thickness is 0.1~0.5mm, and coating weight is 45~50g/m2, the mass fraction of formalin is 25%, and soaking time is
10~15min, control hot pressing pressure are 4~5MPa, and hot pressing temperature is 50~55 DEG C, and hot pressing time is 2~3min.
The beneficial effects of the invention are as follows：
（1）The present invention under conditions of sodium methoxide and catalyst compounded triethanolamine with glycerine by epoxidized soybean oil catalyzed alcoholysis,
Alcoholysis soybean oil is obtained, addition hexamethylene diisocyanate, diethyl phosphate, maleic anhydride into alcoholysis soybean oil, the raw materials such as glycerine,
Polyurethane foam is obtained, ammonium polyphosphate is dissolved in absolute ethyl alcohol, adjusting pH with ammonium hydroxide obtains alkalization flame-proof material, fire-retardant to alkalizing
Methyltriethoxysilane is added in material, filtered after heating reaction, be dried to obtain Silica hydrogel microencapsulation ammonium polyphosphate, silicon is coagulated
Glue microencapsulation ammonium polyphosphate obtains fire retardant adhesive with soybean albumen adhesive mixed preparing, is finally coated with fire retardant adhesive
In the single side of PVC film, polyurethane foam is added between the PVC film that two panels is coated with fire retardant adhesive, obtains composite membrane,
Composite membrane is finally put into hot pressing in hot press and obtains food packaging fire-retardant bubble chamber film, epoxidized soybean oil is due to tool in the present invention
There are good heat resistance, low temperature flexibility, and volatility is low, it is harmless nontoxic, it is environmentally protective, it is widely used, especially suitable for food
It is used as plasticizer in product and drug plastic package material, soybean albumen adhesive used can further be sent out with polyurethane foam
Raw cross-linking reaction makes cementation between polyurethane foam and PVC film enhance, and the epoxy group of epoxidized soybean oil can trap PVC points
The free radical Cl- that son degradation is isolated, terminates the radical reaction of PVC degradations, slows down degradation speed, significantly improve PVC product
Heat resistance assigns the good mechanical strength of product, weatherability, while the low temperature flexibility of epoxidized soybean oil is preferable, to polychlorostyrene second
Alkene has plasticization, and the active chlorine atom in polyvinyl chloride chain can be made to be stablized, and can absorb rapidly because light and heat are degraded
HCl out makes PVC film more stablize, is not easy to discharge noxious material to block the continuous decomposition of polyvinyl chloride, ensures
Health；
（2）Sodium methoxide is a kind of catalyst for ester exchange reaction of highly basic class in the present invention, active very high, sodium methoxide and three ethyl alcohol
The mixed catalyst of amine has good dissolubility in the reaction system, so that reaction is kept homogeneous system, it is anti-can to improve transesterification
The conversion ratio answered obtains the polyurethane foam with polyol structure, and a small amount of p diethylaminobenzoic acid is added when preparing polyurethane foam
Ester, diethyl phosphate are a kind of structures flexible, and diethyl phosphate makes the foam structure of polyurethane foam uniform, uniform to steep
Pore structure makes the mechanical strength of polyurethane foam enhance, and in addition diethyl phosphate can be with the polyol molecule chain of polyurethane foam
It is decomposed during high-temp combustion and generates metaphosphoric acid, metaphosphoric acid makes polyurethane foam be dehydrated and formed on surface in combustion
One layer of close carbon-coating, prevents oxygen and heat to further diffusion inside polyurethane substrates, and the ammonium polyphosphate of anti-flammability is heated
Decomposition can be catalyzed polyurethane and dehydration carburizing reagent occurs, and generate coke layer, and coke layer is fire retardant, have heat-insulated oxygen barrier prevention burning
Effect, make polyurethane foam thermal conductivity be deteriorated, received heat reduce, thermal decomposition rate is slack-off, Silica hydrogel microencapsulation polyphosphoric acid
Element silicon has higher thermal stability in ammonium, will produce stable silicon oxide compound at high temperature, silicon oxide compound is in high temperature
When so that the thermal stability of ammonium polyphosphate is improved, microcapsule structure plays the role of starvation, keeps P elements not oxidized, improves
Thermal stability of the ammonium polyphosphate as fire retardant matter has a wide range of applications to make the flame retardant property of foam film be improved
Foreground.
Specific implementation mode
200~220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is with mass fraction
40% sodium hydroxide solution adjusts pH to 9~10, is heated to 90~100 DEG C to four-hole boiling flask, 60~70g soybean is added
Powder after 50~55min of isothermal holding, 10~12g phenol is added into four-hole boiling flask, is cooled to 70~75 DEG C, isothermal holding 15
~20min continues that 20~25mL formaldehyde is added into four-hole boiling flask, reacts 1~2h, and cooled to room temperature obtains soybean egg
White glue stick；70~80mL epoxidized soybean oils, 4~5g methanol are added into the three-necked flask with dropping funel and condensing unit
Sodium, 5~7mL triethanolamines are heated to 50~60 DEG C, start blender and are stirred with the rotating speed of 200~300r/min,
40~50mL glycerine is added into three-necked flask, insulated and stirred reacts 3~4h, obtains alcoholysis soybean oil；To above-mentioned three-necked flask
Middle addition 80~90mL hexamethylene diisocyanates, 8~10mL styrene the reaction was continued 2~3h, wait for that three-necked flask is cooled to 50~60
DEG C, 10~15mL diethyl phosphates, 20~30mL glycerine and 20~25mL maleic anhydrides is added into three-necked flask successively, separately takes
3~5mL dibutyl tin laurates pour into after being dissolved in 35~40mL acetone in constant pressure funnel, with the dropwise addition of 2~3mL/min
Rate instills in three-necked flask, heats up when being added dropwise, and control heating rate is 3~5 DEG C/min, is warming up to 80~82 DEG C, continues
3~4h is reacted, polyurethane foam is obtained；100~120g ammonium polyphosphate, 230~250mL absolute ethyl alcohols, 100 are added into beaker
~120mL distilled water, is stirred 20~25min, be added into beaker the ammonium hydroxide that mass fraction is 35% adjust pH be 10.2~
10.4, obtain alkalization flame-proof material；20~25g methyltriethoxysilane is added into alkalization flame-proof material, to beaker heating water bath
45~60 DEG C, 2~3h of insulation reaction are warming up to, filtering removal filtrate obtains gel, gel is washed with distilled water 2~3 times
Afterwards, it is put into baking oven, is heated to 80~90 DEG C, dry 5~6h obtains Silica hydrogel microencapsulation ammonium polyphosphate；By soybean
Protein adhesive is that 5 ︰ 1 are mixed to get fire retardant adhesive in mass ratio with Silica hydrogel microencapsulation ammonium polyphosphate, by retardant adhesive
Agent is coated on the single side for the PVC film that thickness is 0.1~0.5mm, and coating weight is 45~50g/m2, polyurethane foam is put into matter
It measures and impregnates 10~15min in the formalin that score is 25%, be put into two panels as interlayer after taking-up and be coated with fire retardant adhesive
Between PVC film, composite membrane is obtained, composite membrane is put into 2~3min of hot pressing in hot press, control hot pressing pressure is 4~5MPa,
Hot pressing temperature is 50~55 DEG C, obtains food packaging fire-retardant bubble chamber film.
200mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is 40% with mass fraction
Sodium hydroxide solution adjusts pH to 9, and 90 DEG C are heated to four-hole boiling flask, is added 60g soy meals, after isothermal holding 50min,
10g phenol is added into four-hole boiling flask, is cooled to 70 DEG C, isothermal holding 15min, continues that 20mL first is added into four-hole boiling flask
Aldehyde, reacts 1h, and cooled to room temperature obtains soybean albumen adhesive；To three mouthfuls of burnings with dropping funel and condensing unit
70mL epoxidized soybean oils, 4g sodium methoxides, 5mL triethanolamines are added in bottle, is heated to 50 DEG C, starts blender with 200r/
The rotating speed of min is stirred, and 40mL glycerine is added into three-necked flask, and insulated and stirred reacts 3h, obtains alcoholysis soybean oil；Upwards
Stating in three-necked flask addition 80mL hexamethylene diisocyanates, 8mL styrene the reaction was continued 2h waits for that three-necked flask is cooled to 50 DEG C, according to
It is secondary that 10mL diethyl phosphates, 20mL glycerine and 20mL maleic anhydrides are added into three-necked flask, separately take 3mL di lauric dibutyls
Tin pours into after being dissolved in 35mL acetone in constant pressure funnel, is instilled in three-necked flask with the drop rate of 2mL/min, when being added dropwise
Heating, control heating rate are 3 DEG C/min, are warming up to 80 DEG C, and the reaction was continued 3h obtains polyurethane foam；It is added into beaker
100g ammonium polyphosphate, 230mL absolute ethyl alcohols, 100mL distilled water, are stirred 20min, and mass fraction is added into beaker and is
It is 10.2 that 35% ammonium hydroxide, which adjusts pH, obtains alkalization flame-proof material；20g methyltriethoxysilane is added into alkalization flame-proof material, it is right
Beaker water-bath is heated to 45 DEG C, insulation reaction 2h, and filtering removal filtrate obtains gel, gel is washed with distilled water 2 times
Afterwards, it is put into baking oven, is heated to 80 DEG C, dry 5h obtains Silica hydrogel microencapsulation ammonium polyphosphate；By soybean protein gluing
Agent is that 5 ︰ 1 are mixed to get fire retardant adhesive in mass ratio with Silica hydrogel microencapsulation ammonium polyphosphate, and fire retardant adhesive is coated on
Thickness is the single side of the PVC film of 0.1mm, coating weight 45g/m2, polyurethane foam is put into the formaldehyde that mass fraction is 25%
10min is impregnated in solution, is put between two panels is coated with the PVC film of fire retardant adhesive, is obtained compound as interlayer after taking-up
Composite membrane is put into hot pressing 2min in hot press by film, and control hot pressing pressure is 4MPa, and hot pressing temperature is 50 DEG C, obtains food packet
Fill fire-retardant bubble chamber film.
210mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is 40% with mass fraction
Sodium hydroxide solution adjusts pH to 9.5, is heated to 95 DEG C to four-hole boiling flask, 65g soy meals, isothermal holding 53min is added
Afterwards, 11g phenol is added into four-hole boiling flask, is cooled to 73 DEG C, isothermal holding 17min continues that 23mL is added into four-hole boiling flask
Formaldehyde, reacts 1.5h, and cooled to room temperature obtains soybean albumen adhesive；To three with dropping funel and condensing unit
75mL epoxidized soybean oils, 4.5g sodium methoxides, 6mL triethanolamines are added in mouthful flask, is heated to 55 DEG C, start blender with
The rotating speed of 250r/min is stirred, and 45mL glycerine is added into three-necked flask, and insulated and stirred reacts 3.5h, obtains alcoholysis soybean
Oil；85mL hexamethylene diisocyanates are added into above-mentioned three-necked flask, 9mL styrene the reaction was continued 2.5h waits for that three-necked flask cools down
To 55 DEG C, 13mL diethyl phosphates, 25mL glycerine and 23mL maleic anhydrides is added into three-necked flask successively, separately takes 4mL February
Dilaurylate pours into after being dissolved in 38mL acetone in constant pressure funnel, and three mouthfuls of burnings are instilled with the drop rate of 2.5mL/min
In bottle, heat up when being added dropwise, control heating rate is 4 DEG C/min, is warming up to 81 DEG C, and the reaction was continued 3.5h obtains polyurethane foam
Foam；110g ammonium polyphosphate, 240mL absolute ethyl alcohols, 110mL distilled water are added into beaker, 23min is stirred, into beaker
It is 10.3 that the ammonium hydroxide that mass fraction is 35%, which is added, and adjusts pH, obtains alkalization flame-proof material；23g methyl is added into alkalization flame-proof material
Triethoxysilane is heated to 53 DEG C, insulation reaction 2.5h to beaker water-bath, and filtering removal filtrate obtains gel, will coagulate
It after glue is washed with distilled water 2 times, is put into baking oven, is heated to 85 DEG C, dry 5.5h obtains the poly- phosphorus of Silica hydrogel microencapsulation
Sour ammonium；It is that 5 ︰ 1 are mixed to get fire retardant adhesive in mass ratio by soybean albumen adhesive and Silica hydrogel microencapsulation ammonium polyphosphate,
Fire retardant adhesive is coated on to the single side for the PVC film that thickness is 0.3mm, coating weight 47g/m2, polyurethane foam is put into
13min is impregnated in the formalin that mass fraction is 25%, being put into two panels as interlayer after taking-up is coated with fire retardant adhesive
Between PVC film, composite membrane is obtained, composite membrane is put into hot pressing 2.5min in hot press, control hot pressing pressure is 4.5MPa, heat
It is 53 DEG C to press temperature, obtains food packaging fire-retardant bubble chamber film.
220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is 40% with mass fraction
Sodium hydroxide solution adjusts pH to 10, is heated to 100 DEG C to four-hole boiling flask, 70g soy meals, isothermal holding 55min is added
Afterwards, 12g phenol is added into four-hole boiling flask, is cooled to 75 DEG C, isothermal holding 20min continues that 25mL is added into four-hole boiling flask
Formaldehyde, reacts 2h, and cooled to room temperature obtains soybean albumen adhesive；To three mouthfuls with dropping funel and condensing unit
80mL epoxidized soybean oils, 5g sodium methoxides, 7mL triethanolamines are added in flask, is heated to 60 DEG C, start blender with
The rotating speed of 300r/min is stirred, and 50mL glycerine is added into three-necked flask, and insulated and stirred reacts 4h, obtains alcoholysis soybean
Oil；90mL hexamethylene diisocyanates are added into above-mentioned three-necked flask, 10mL styrene the reaction was continued 3h waits for that three-necked flask is cooled to
60 DEG C, 15mL diethyl phosphates, 30mL glycerine and 25mL maleic anhydrides is added into three-necked flask successively, separately takes bis- bays of 5mL
Sour dibutyl tin pours into after being dissolved in 40mL acetone in constant pressure funnel, is instilled in three-necked flask with the drop rate of 3mL/min,
Heat up when being added dropwise, control heating rate is 5 DEG C/min, is warming up to 82 DEG C, and the reaction was continued 4h obtains polyurethane foam；To burning
120g ammonium polyphosphate, 250mL absolute ethyl alcohols, 120mL distilled water are added in cup, is stirred 25min, quality is added into beaker
It is 10.4 that the ammonium hydroxide that score is 35%, which adjusts pH, obtains alkalization flame-proof material；25g methyl triethoxies are added into alkalization flame-proof material
Silane is heated to 60 DEG C, insulation reaction 3h to beaker water-bath, and filtering removal filtrate obtains gel, by gel distilled water
It after washing 3 times, is put into baking oven, is heated to 90 DEG C, dry 6h obtains Silica hydrogel microencapsulation ammonium polyphosphate；By soybean
Protein adhesive is that 5 ︰ 1 are mixed to get fire retardant adhesive in mass ratio with Silica hydrogel microencapsulation ammonium polyphosphate, by retardant adhesive
Agent is coated on the single side for the PVC film that thickness is 0.5mm, coating weight 50g/m2, polyurethane foam, which is put into mass fraction, is
15min is impregnated in 25% formalin, is put between two panels is coated with the PVC film of fire retardant adhesive as interlayer after taking-up,
Composite membrane is obtained, composite membrane is put into hot pressing 3min in hot press, control hot pressing pressure is 5MPa, and hot pressing temperature is 55 DEG C, is obtained
To food packaging fire-retardant bubble chamber film.
The bubble chamber film that comparative example is produced with company of Suzhou City is as a comparison case
Bubble chamber film in food packaging fire-retardant bubble chamber film produced by the present invention and comparative example is detected, testing result such as table
Shown in 1：
1, Mechanics Performance Testing
It is carried out according to standard GB/T1040.3-2006, rate of extension 200mm/min, sensor 500N.
Chloride content is tested in food
With reference to GB5009.44-2016《The measurement of chloride in national food safety standard food》It is tested.
1 performance measurement result of table
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example |
| Tensile strength（MPa） | 31.2 | 32.8 | 33.4 | 9.7 |
| Elongation at break（%） | 564.3 | 565.2 | 566.6 | 451.2 |
| Density（kg/m3） | 18.5 | 18.4 | 18.2 | 24.5 |
| Water absorption rate（kg/m2） | 0.007 | 0.006 | 0.006 | 0.012 |
| Moisture-vapor transmission（g/m2·h） | 0.008 | 0.007 | 0.006 | 0.011 |
| Natural degradation time（d） | 45 | 43 | 40 | It can not degrade |
| Oxygen index (OI) | 31 | 33 | 34 | 20 |
| Horizontal firing length（mm） | 5 | 4 | 3 | 20 |
| The vertical combustion time（s） | 0 | 0 | 0 | 1 |
| Chlorinity（mg/kg） | 0.02 | 0.01 | 0.01 | 0.35 |
From the data in table 1, it can be seen that food packaging fire-retardant bubble chamber film produced by the present invention, have light, intensity is high, it is fire-retardant, moisture-proof,
The features such as shockproof, while can degrade, it is good for the environment.Present invention process is advanced, and production method is simple and fast efficiently, has good
Good market prospects.
Claims (7)
1. a kind of preparation method of food packaging fire-retardant bubble chamber film, it is characterised in that specifically preparation process is：
（1）200~220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, uses sodium hydroxide solution
PH is adjusted, to four-hole boiling flask heat temperature raising, is added 60~70g soy meals, after isothermal holding, it is added 10 into four-hole boiling flask~
12g phenol, cooling, isothermal holding continue that 20~25mL formaldehyde is added into four-hole boiling flask, and reaction, cooled to room temperature obtains
To soybean albumen adhesive；
（2）70~80mL epoxidized soybean oils, 4~5g methanol are added into the three-necked flask with dropping funel and condensing unit
Sodium, 5~7mL triethanolamines, heat temperature raising are started blender and are stirred with the rotating speed of 200~300r/min, to three-necked flask
Middle addition 40~50mL glycerine, insulated and stirred reaction, obtains alcoholysis soybean oil；
（3）80~90mL hexamethylene diisocyanates are added into above-mentioned three-necked flask, the reaction was continued for 8~10mL styrene, waits for three mouthfuls
Flask cools down, and 10~15mL diethyl phosphates, 20~30mL glycerine and 20~25mL maleic acids is added into three-necked flask successively
Acid anhydride pours into after separately taking 3~5mL dibutyl tin laurates to be dissolved in 35~40mL acetone in constant pressure funnel, then instills three mouthfuls
In flask, heat up when being added dropwise, the reaction was continued, obtains polyurethane foam；
（4）100~120g ammonium polyphosphate, 230~250mL absolute ethyl alcohols, 100~120mL distilled water, stirring are added into beaker
Ammonium hydroxide adjusting pH is added into beaker, obtains alkalization flame-proof material for mixing；
（5）20~25g methyltriethoxysilane is added into alkalization flame-proof material, to beaker water-bath heat temperature raising, insulation reaction,
Filtering removal filtrate, obtains gel, after gel is washed with distilled water 2~3 times, is put into baking oven, heat temperature raising, dry, obtains
To Silica hydrogel microencapsulation ammonium polyphosphate；
（6）Soybean albumen adhesive and Silica hydrogel microencapsulation ammonium polyphosphate are mixed to get fire retardant adhesive, by retardant adhesive
Agent is coated on the single side of PVC film, and polyurethane foam is put into formalin and is impregnated, and being put into two panels as interlayer after taking-up applies
It is furnished between the PVC film of fire retardant adhesive, obtains composite membrane, composite membrane is put into hot pressing in hot press, obtains food packaging
With fire-retardant bubble chamber film.
2. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：
Step（1）The mass fraction of the sodium hydroxide solution is 40%, and it is 9~10 to adjust pH with sodium hydroxide solution, to four
Temperature is 90~100 DEG C after mouth flask heat temperature raising, and the isothermal holding time is 50~55min after heating, and temperature is 70 after cooling
~75 DEG C, the isothermal holding time is 15~20min after cooling, and the reaction time is 1~2h.
3. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：
Step（2）Temperature is 50~60 DEG C after the heat temperature raising, and agitator speed is 200~300r/min, insulated and stirred
Reaction time is 3~4h.
4. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：
Step（3）The styrene the reaction was continued time is 2~3h, and temperature is 50~60 DEG C after three-necked flask cooling, constant pressure
Dropping funel drop rate is 2~3mL/min, and control heating rate is 3~5 DEG C/min, and temperature is 80~82 DEG C after heating, after
The continuous reaction time is 3~4h.
5. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：
Step（4）Described to be stirred the time as 20~25min, the mass fraction of ammonium hydroxide is 35%, and ammonium hydroxide tune is added into beaker
It is 10.2~10.4 to save pH.
6. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：
Step（5）Described is 45~60 DEG C to temperature after beaker water-bath heat temperature raising, and the insulation reaction time is 2~3h, baking oven
Temperature is 80~90 DEG C after heat temperature raising, and drying time is 5~6h.
7. a kind of preparation method of food packaging fire-retardant bubble chamber film according to claim 1, it is characterised in that：Step
（6）The soybean albumen adhesive is 5 ︰ 1 with Silica hydrogel microencapsulation ammonium polyphosphate mixing quality ratio, and PVC film thickness is
0.1~0.5mm, coating weight are 45~50g/m2, the mass fraction of formalin is 25%, and soaking time is 10~15min, control
Heating pressure pressure is 4~5MPa, and hot pressing temperature is 50~55 DEG C, and hot pressing time is 2~3min.
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| CN117364487A (en) * | 2023-12-04 | 2024-01-09 | 江苏恒力化纤股份有限公司 | Preparation method of durable flame-retardant coating polyester/cotton blended fabric |
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