CN105524332A - Production process of fresh-keeping film based on titanium dioxide - Google Patents

Production process of fresh-keeping film based on titanium dioxide Download PDF

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Publication number
CN105524332A
CN105524332A CN201610076411.8A CN201610076411A CN105524332A CN 105524332 A CN105524332 A CN 105524332A CN 201610076411 A CN201610076411 A CN 201610076411A CN 105524332 A CN105524332 A CN 105524332A
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titanium dioxide
film
fresh
production technique
keeping
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CN201610076411.8A
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Chinese (zh)
Inventor
张川
张千
***
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HEBEI MILSON TITANIUM DIOXIDE CO Ltd
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HEBEI MILSON TITANIUM DIOXIDE CO Ltd
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Priority to CN201610076411.8A priority Critical patent/CN105524332A/en
Publication of CN105524332A publication Critical patent/CN105524332A/en
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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
    • C08K9/10—Encapsulated ingredients
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • 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
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • 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
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • 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
    • 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
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/066—LDPE (radical process)

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

The invention relates to a production process of a fresh-keeping film based on titanium dioxide. The production process comprises preparation of a film material from raw materials including titanyl sulfate and clear lime water and preparation of a film product from the film material, wherein the clear lime water is used for neutralizing acidity of titanyl sulfate, titanyl sulfate is hydrolyzed to generate nano titanium dioxide containing metatitanic acid, nano titanium dioxide containing metatitanic acid is subjected to spray drying, nano titanium dioxide particles are obtained, ground by gas stream and organically coated with films, a preparation raw material for the fresh-keeping film is formed, the modified nano titanium dioxide particles are subjected to master batch granulation through a double-screw extruder, mother batch is melt through a single-screw extruder, and finally, film casting is performed. A finished product of the fresh-keeping film has the advantages of uniform ingredients, uniform surface structure, no pin holes, good stability and the like, and the nano fresh-keeping film has excellent fresh-keeping performance, and the fresh-keeping degree of fruits and vegetables is greatly improved.

Description

A kind of production technique of the antistaling film based on titanium dioxide
Technical field
The invention belongs to food fresh keeping thin film fabrication techniques field, be specifically related to a kind of production technique of the antistaling film based on titanium dioxide.
Background technology
Because weather had four seasons samsara in the middle of 1 year, there is specific seasonality as fruits and vegetables.In the busy season, rich choice of products, price is lower; In the dull season, supply is rare, and price is higher, there is significantly seasonal and price difference ratio.Although along with agrotechnical raising, the vegetables of anti-season plantation grow a lot, the vast northern area that, temperature long for winter is low, and anti-season plantation power consumption is large, and cost is high, and mainly or by storage regulates supply in dull season for most of fruit.Therefore, research and develop satisfactory for result, with low cost, easy to operate postharvest technology of fruits and vegetables, not only can improve the standard of living of people, and significant economic benefit and social benefit can also be received.
The technique means adopted in field of food preservation both at home and abroad mainly contains the large class of physics and chemistry two, and the new technology that each class derives is a lot, relies on different fresh keeping principles separately.Various preservation technique is all that the three large key elements by playing a crucial role to preservation quality regulate and control: first, is to control its senescence process, generally by realizing respiratory control; Secondly, microorganism is controlled, mainly through realizing the control of spoilage organism; 3rd, control internal moisture evaporation, mainly through realizing the control of ambient relative humidity and the structurizing of iuntercellular moisture.
Summary of the invention
For the shortcoming of the fresh-keeping effect difference of preservative film in prior art, the invention provides a kind of production technique of the antistaling film based on titanium dioxide, the antistaling film fresh keeping time that this production technique is produced is long, effect stability, and smooth surface, tensile strength is good, not cracky.
Concrete technical scheme of the present invention:
Based on a production technique for the antistaling film of titanium dioxide, key point is, this production technique comprises with titanyl sulfate and clarifies liming for raw materials in producing films material and process thin-film material preparation being formed finished film, and this process mainly comprises the following steps:
The preparation of thin-film material:
A1, by titanyl sulfate with clarification liming mix, blending ratio for can make mixed solution pH value between 5.5-7.5, mixing after acquisition particle diameter be the anatase titanium dioxide of 20-50nm;
B1, drying is carried out to titanium dioxide;
C1, dried titanium dioxide to be pulverized, and carry out coating in crushing process, finally form thin-film material;
The preparation of film:
A2, by TiO 2 particles and LDPE resin Homogeneous phase mixing, be then delivered to twin screw extruder and carry out granulation, form master batch;
B2, master batch is sent into single screw extrusion machine melt extrude and carry out casting film-forming through sharp cooling roll and wind-up roll, finally form antistaling film finished product.
In described steps A 1, titanyl sulfate and clarification liming carry out high speed dispersion mixing, and the titanium dioxide particle diameter generated after mixing is between 20-50nm, and the speed of high speed dispersion is 18000r/min.
In described step B1, dry equipment used is spray-drier.
In described step C1, pulverizing equipment used is micronizer mill, adds organosilicon and carry out coating to titanium dioxide in crushing process.
Described organosilyl addition is 0.5% of titanium dioxide quality.
In described steps A 2, the screw speed of twin screw extruder is 300r/min, and be followed successively by 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C by feed end to four sections of temperature of die head, input speed is 1.5kg/h.
In described step B2, the screw speed of single screw extrusion machine is 40r/min, 200 DEG C, 200 DEG C, 200 DEG C, 210 DEG C are followed successively by four sections of temperature of die head by feed end, one group of described sharp cooling roll quantity is six, is followed successively by 50r/min, 60r/min, 70r/min, 100r/min, 100r/min, 100r/min by near-lying mode head end to the rotating speed of the sharp cooling roll away from die end.
The invention has the beneficial effects as follows: this film adopts titanyl sulfate and liming to carry out the production of film as raw material, both are meeting generating portion calcium sulfate in N-process, calcium sulfate is a kind of plant preservation agent efficiently, and grain diameter as film raw material in present invention process is less, and extra-granular carries out organosilicon coating, avoid reunion, roughness obviously declines, the anti-water vapour permeability of film produced is strong, tensile strength is high, frictional coefficient is little, utilize this antistaling film can increase the fresh keeping time of plant, and fresh-keeping effect is comparatively stable.
Embodiment
The present invention relates to a kind of production technique of the antistaling film based on titanium dioxide, this production technique comprises with titanyl sulfate and clarifies liming for raw materials in producing films material and process thin-film material preparation being formed finished film.
Specific embodiment, carry out fresh-keeping to the antistaling film that needle mushroom adopts production technique of the present invention to obtain, the concrete steps of production technique are as described below:
The preparation of thin-film material:
Under A1, normal temperature, by the titanyl sulfate of decon process and clarification liming stream adds in mulser, throughput ratio is that the pH value of liquid in control mulser is between 5.5-7.5, till the theoretical concentration that titanyl sulfate and liming continue to add titanium dioxide in emulsifying tank is 50g/L, the rotating speed of mulser is not less than 18000r/min, the Fe < 30 × 10 in titanyl sulfate used 6under high speed dispersion condition, by the acidity of clarification liming neutralisation of sulphuric acid oxygen titanium, titanyl sulfate is hydrolyzed and generates nano titanium oxide, the effect of high speed dispersion makes the particle diameter of titanium dioxide can not be excessive, and the titanium dioxide particle diameter having neutralized rear generation, between 20-50nm, is anatase titanium dioxide, have nanometer calcium sulfate during neutralization to generate, the nano titanium oxide of this calcic is a kind of plant preservation agent efficiently;
Metatitanic acid hydrolyzed solution after B1, hydrolysis, main component is hydrated titanium dioxide, is sent spray-drier dry, prepares nano titanium oxide.
C1, dried titanium dioxide to be pulverized, equipment used is micronizer mill, the process of comminution by gas stream is soft-agglomerated in order to thoroughly open the titanium dioxide formed in drying process, and in order to prevent the soft-agglomerated of nano titanium oxide, adopt nanometer titanium dioxide silicone content be 15% organosilicon carry out organic coated dispersion, organosilyl addition is 0.5%, finally forms the nano titanium oxide of dispersion, prepares material as film;
The preparation of film:
A2, first to mix in high-speed mixer with LDPE resin through modified nano-titania particle, then by twin screw extruder extruding pelletization, test conditions is set as follows: screw speed is 300r/min, 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C are followed successively by four sections of temperature of die head by feed end, input speed controls, at about 1.5kg/h, finally to obtain master batch;
B2, gained master batch extrudes casting film-forming through single screw extrusion machine, with single screw extrusion machine, master batch raw material is melted, screw speed is 40r/min, 200 DEG C are followed successively by four sections of temperature of die head by feed end, 200 DEG C, 200 DEG C, 210 DEG C, there are volume pump and mould in head place, in front end, master batch material extruding place, heating guide roll is set, heating deflector roll temperature is 90 DEG C, carry out the preheating of master batch raw material, through one group of sharp cooling roll after being extruded by die lip, 50r/min is followed successively by the rotating speed of the sharp cooling roll away from die end by near-lying mode head end, 60r/min, 70r/min, 100r/min, 100r/min, 100r/min, and then form finished product through wind-up roll traction, wind-up roll rotating speed is 30r/min.Nano modification film thickness obtained under above-mentioned condition is 40 ± 2 μm, meets the thickness range of most of polyethylene antistaling film packaging 30-50 μm.
The antistaling film that production technique of the present invention is produced, principal character be have good fresh-keeping, antioxygen, aseptic, protect fragrant, oil resistant, the feature such as transparent, by infrared, the structure of scanning electron microscope to natural complex fresh-keeping film is analyzed, find the Si in film, Ca, Ti presents comparatively regularly arranged labyrinth structure, water vapour permeability, tensile strength and frictional behaviour test show, compared with pure PP, the rate of perviousness of composite fresh-keeping film reduces, tensile strength increases, rubbing factor reduces, this antistaling film is utilized to pack needle mushroom, needle mushroom is at unglazed photograph, temperature is lower than when preserving the 23rd day under the condition of 20 DEG C, rate of weight loss is 6.5%, rotting mechanism is 19%, organic acid mass content is 0.25%, vitamins C (Vc) mass content is 0.72mg/g, fresh-keeping effect is excellent.
In the present invention the complete processing of film have uniform component, surface tissue evenly, the advantage such as free of pinholes, good stability, therefore, the fresh keeping property of this nanometer antistaling film is excellent, substantially increases the freshness of fruits and vegetables.

Claims (7)

1. the production technique based on the antistaling film of titanium dioxide, it is characterized in that: this production technique comprises with titanyl sulfate and clarifies liming for raw materials in producing films material and process thin-film material preparation being formed finished film, and this process mainly comprises the following steps:
The preparation of thin-film material:
A1, by titanyl sulfate with clarification liming mix, blending ratio for can make mixed solution pH value between 5.5-7.5, mixing after acquisition particle diameter be the anatase titanium dioxide of 20-50nm;
B1, drying is carried out to titanium dioxide;
C1, dried titanium dioxide to be pulverized, and carry out coating in crushing process, finally form thin-film material;
The preparation of film:
A2, by TiO 2 particles and LDPE resin Homogeneous phase mixing, be then delivered to twin screw extruder and carry out granulation, form master batch;
B2, master batch is sent into single screw extrusion machine melt extrude and carry out casting film-forming through sharp cooling roll and wind-up roll, finally form antistaling film finished product.
2. the production technique of a kind of antistaling film based on titanium dioxide according to claim 1, it is characterized in that: in described steps A 1, titanyl sulfate and clarification liming carry out high speed dispersion mixing, the titanium dioxide particle diameter generated after mixing is between 20-50nm, and the speed of high speed dispersion is 18000r/min.
3. the production technique of a kind of antistaling film based on titanium dioxide according to claim 1, is characterized in that: in described step B1, and dry equipment used is spray-drier.
4. the production technique of a kind of antistaling film based on titanium dioxide according to claim 1, is characterized in that: in described step C1, and pulverizing equipment used is micronizer mill, adds organosilicon and carry out coating to titanium dioxide in crushing process.
5. the production technique of a kind of antistaling film based on titanium dioxide according to claim 4, is characterized in that: described organosilyl addition is 0.5% of titanium dioxide quality.
6. the production technique of a kind of antistaling film based on titanium dioxide according to claim 1, it is characterized in that: in described steps A 2, the screw speed of twin screw extruder is 300r/min, be followed successively by 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C by feed end to four sections of temperature of die head, input speed is 1.5kg/h.
7. the production technique of a kind of antistaling film based on titanium dioxide according to claim 1, it is characterized in that: in described step B2, the screw speed of single screw extrusion machine is 40r/min, 200 DEG C, 200 DEG C, 200 DEG C, 210 DEG C are followed successively by four sections of temperature of die head by feed end, one group of described sharp cooling roll quantity is six, is followed successively by 50r/min, 60r/min, 70r/min, 100r/min, 100r/min, 100r/min by near-lying mode head end to the rotating speed of the sharp cooling roll away from die end.
CN201610076411.8A 2016-02-03 2016-02-03 Production process of fresh-keeping film based on titanium dioxide Pending CN105524332A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106916367A (en) * 2017-03-16 2017-07-04 华南理工大学 A kind of film containing nano titanium oxide and preparation method thereof
CN107641300A (en) * 2017-10-09 2018-01-30 常州美帛纺织品有限公司 A kind of preparation method of vapor-permeable type polyethylene terephthalate thin film
CN109527069A (en) * 2018-12-25 2019-03-29 杭州宝积生物科技有限公司 A kind of novel fresh egg product photocatalyst Non-water washing bactericidal cleaning fresh-keeping liquid and birds, beasts and eggs
CN112830463A (en) * 2021-01-15 2021-05-25 南京尚迪纳米科技有限公司 Preparation method and application of nano fresh-keeping material

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CN102875868A (en) * 2012-09-11 2013-01-16 大连巨峰包装制品有限公司 Method for preparing food fresh-keeping film
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106916367A (en) * 2017-03-16 2017-07-04 华南理工大学 A kind of film containing nano titanium oxide and preparation method thereof
CN106916367B (en) * 2017-03-16 2019-04-09 华南理工大学 A kind of film and preparation method thereof containing nano-titanium dioxide
CN107641300A (en) * 2017-10-09 2018-01-30 常州美帛纺织品有限公司 A kind of preparation method of vapor-permeable type polyethylene terephthalate thin film
CN109527069A (en) * 2018-12-25 2019-03-29 杭州宝积生物科技有限公司 A kind of novel fresh egg product photocatalyst Non-water washing bactericidal cleaning fresh-keeping liquid and birds, beasts and eggs
CN112830463A (en) * 2021-01-15 2021-05-25 南京尚迪纳米科技有限公司 Preparation method and application of nano fresh-keeping material

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