CN106380731A - PVC film for wallpaper and preparation method thereof - Google Patents
PVC film for wallpaper and preparation method thereof Download PDFInfo
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- CN106380731A CN106380731A CN201610781338.4A CN201610781338A CN106380731A CN 106380731 A CN106380731 A CN 106380731A CN 201610781338 A CN201610781338 A CN 201610781338A CN 106380731 A CN106380731 A CN 106380731A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
- C08F220/325—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals containing glycidyl radical, e.g. glycidyl (meth)acrylate
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- 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
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2203/14—Applications used for foams
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- C08L2203/16—Applications used for films
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a PVC film for wallpaper and a preparation method thereof. The preparation method comprises the following steps: adding all raw materials and reagents in proportion into a high speed mixer and mixing for 5-8 min so as to obtain a premix material; carrying out melt extrusion by a double screw extruder to form battens, and crushing by a pulverizer; and carrying out injection moulding by the use of an injection moulding machine so as to obtain the PVC film for wallpaper. Raw materials and reagents of the PVC film contain a raw material polyvinyl chloride, carbon fiber, a Pb-Ba stabilizing agent, paraffin, stearic acid, glycidyl methacrylate, maleic anhydride, acrylic acid, dicumyl peroxide, bis(1-(tert-butylperoxy)-1-methylethyl)-benzene, benzoyl peroxide, di-tert-butylperoxide, styrene, epoxy resin E-44 and MgO nano-particles and nano-copper powder colloid. The PVC material has excellent fireproofness and good toughness, and is not easy for tensile failure.
Description
Technical field
The present invention relates to Chemical products technical field, particularly to a kind of wallpaper PVC film and preparation method thereof.
Background technology
Polrvinyl chloride (PVC) was synthesized by Regnault first in 1835, was directed to vinyl chloride monomer polymerization reactions within 1912
The technique generating polrvinyl chloride is applied patent.But the PVC for business must have stability and easy plastify or blending
Ability, therefore, after have passed through researchers' latent also research and development of 15 years and modified optimization, polrvinyl chloride is just formally commercialized.
Because PVC has the advantages that nonflammable, corrosion-resistant, insulation, wear-resistant, and preparation process is simple, abundant raw materials, price
Cheap, PVC is also pursued by businessman and consumer therefore and deeply.
The big resins for universal use of China five is respectively polyethylene（PE）, polypropylene（PP）, polystyrene（PS）, acrylic nitrile-butadiene two
Alkene-styrol copolymer（ABS）, polrvinyl chloride（PVC）.PVC as the plastics of yield second in five big resins for universal use, due to
Its excellent cost performance, is widely used in various fields.PVC particularly may be divided into two parts.A part is flexible PVC material
Material, is mainly used in cable, artificial leather, all kinds of flexible pipe, plastic shoes etc.；Another part is hard PVC material, and referring mainly to should
For all kinds of sheet material section bars of industry such as building etc..Wherein, China improves constantly in hard product consumption proportion, now close
60%, roughly the same with global PVC hard product consumption proportion.
But PVC heat stability and shock resistance are poor.On open market and indication of the present invention polyvinyl chloride resin actually
Refer to add the blend of each analog assistant in pure PVC resin.
Its surface of PVC wallpaper mainly adopts Corvic, mainly has following three kinds：
, with the paper of 80g/ square meter as paper substrate, surface applies 100g/ square meter polyvinyl chloride resin for A, plain edition --- ---.Its incrustation
Method is usually stamp, embossing or stamp and combining of being embossed.
B, expansion type --- ----and with the paper of 100g/ square meter as paper substrate, surface applies the polyvinyl chloride resin of 300-400g/ square meter.
By the size of expansion ratio, there is the difference of low ratio foamed and high-foaming again.The wherein whippy concavo-convex flower of high-foaming wallpaper surface
Stricture of vagina, has certain acoustically effective.
C, functional type --- --- are wherein water-fast, and wallpaper is to make base material with glass fabric, can be used for decorating toilet, bathroom
Metope；It is base material that fireproof wallpaper then adopts the asbestos paper of 100-200g/ square meter, and mixes fire retardant in PVC facestock.
PVC wallpaper has certain water proofing property, easy construction.After surface contamination, clean sponge or towel is can use to wipe.Root
According to the difference of its water proofing property, it is divided into following two again：
(1) PVC coating wallpaper（With pure paper, non-woven fabrics or spinning cloth as base material）
With pure paper, non-woven fabrics, spin cloth etc. as base material, spray PVC paste shape resin in substrate surface, then through operations such as stamp, embossing
Process.
This kind of wallpaper can produce very strong three-dimensional stereopsis after foaming process, and can be fabricated to various stricture of vaginas true to nature
Reason effect, such as imitation wood stricture of vagina, imitative damask, imitative ceramic tile etc., have stronger texture and preferable breathability, can preferably resist oils and fatss
With the erosion of dampness, can be used on kitchen and toilet, be suitable for nearly all household place.
(2) PVC glue surface wallpaper（With pure paper or fabric as base material）
Such wallpaper is in pure paper bottom（Or non-woven fabrics, spinning cloth bottom）Upper covering one strata vinyl chloride film, through being combined, being embossed,
The operations such as stamp are made.Such wallpaper stamp is exquisite, good, durable in use, the easy maintenance of embossing good texture, waterproof and dampproof property is protected
Support.This kind of wallpaper is wallpaper the most frequently used at present, that purposes is the widest, can be widely applied to all of household and commercial location.
Content of the invention
The technical problem to be solved is：Provide a kind of wallpaper PVC film and preparation method thereof.The present invention
PVC material has excellent fire protecting performance, and good toughness, unsuitable tension failure.The wallpaper also making is readily cleaned to be arranged, dirty
When, only gently need to be wiped with wet cloth, both cleanable as before, very easily arrange.
For solving above-mentioned technical problem, the invention provides a kind of wallpaper PVC film, the preparation of described wallpaper PVC film
Method is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
The source chemicals of described PVC film include one or more of：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
Described wallpaper PVC film, is made up of the source chemicals of following weight portion：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
Described carbon fiber is PAN base carbon fibre, and described MgO nano-particle is cubic structure, and substantially spherical in shape, its particle diameter is
28-32nm.
Described wallpaper PVC film, can prepare expansion type PVC wallpaper further.
For solving above-mentioned technical problem, present invention also offers a kind of preparation method of wallpaper PVC film, step is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
The source chemicals of described PVC film include one or more of：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
The preparation of described wallpaper PVC film, is made up of the source chemicals of following weight portion：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
Described carbon fiber is PAN base carbon fibre, and described MgO nano-particle is cubic structure, and substantially spherical in shape, its particle diameter is
28-32nm.
For solving above-mentioned technical problem, invention further provides a kind of application of the preparation method of described wallpaper PVC film,
Described wallpaper PVC film, can be further used for preparing expansion type PVC wallpaper.
Beneficial the having technical effect that of the present invention：PVC material of the present invention has excellent fire protecting performance, and good toughness,
Unsuitable tension failure.The wallpaper also making is readily cleaned to be arranged, and when dirty, only gently need to be wiped with wet cloth, both cleanable as before, ten
Partial volume is easily arranged.
Brief description
Fig. 1 is the molding process of hard PVC and flexible PVC described in the embodiment of the present invention；
Fig. 2 is the molding process that PVC described in the embodiment of the present invention pastes plastics.
Specific embodiment
To describe embodiments of the present invention below with reference to embodiment in detail, whereby to the present invention how application technology handss
Section is solving technical problem, and reaches realizing process and fully understanding and implement according to this of technique effect.
It should be noted that writing length for saving description, it is to avoid unnecessary repetition and waste, in the feelings do not conflicted
Under condition, the embodiment in the application and the feature in embodiment can be mutually combined.
The formula of polyvinyl chloride composite materials is primarily referred to as thering is certain characteristic by adjusting the preparation of PVC blend ingredients
PVC material product, improves a class formula of the processing characteristics of PVC resin.Its composition, in addition to Corvic matrix, is gone back
Stabilizer, plasticizer, lubricant, modifying agent, filler, colorant and processing aid etc. need to be added according to the actual requirements.
Stabilizer plays an important role in PVC composite, is mainly used in suppressing the decomposition of PVC, prevents from dropping
Solution.The one big shortcoming of PVC is that heat stability is poor, and its decomposition temperature is less than melt temperature.Therefore, improve decomposition temperature, for
PVC processing is most important.
Plasticizer is mainly used in improving polymer plastic in PVC composite-material formula.Plasticizer can make resin expansion,
It is incorporated in resin, reduces intermolecular gravitation, make resin become soft, reduce the processing temperature of resin, improve composite
Mobility at processing temperatures.
Lubricant is mainly used in reducing friction in PVC composite-material formula.After compound adds extruder, due to
Extrusion shearing, has friction phenomenon between polymer and between polymer and screw rod.Excessive friction can reduce mobility, and
And substantial amounts of heat can be produced and cause the degraded of PVC.Now, the certain effect of lubricant plays.Generally, lubricant
Including in-lubricant and external lubricant, it is respectively used to reduce and rubs between compound internal friction and batch mixing and equipment.
Processing aid is mainly used in improving processing characteristics in PVC composite-material formula.PVC resin is due to thermally-stabilised
Property poor, hardly result in real melt, melt viscosity is big, poor fluidity, can not be conducted heat well between melt, in processing
In be susceptible to melt fracture.Processing aid can promote the melting of PVC, improves mouldability of PVC etc..Conventional processing helps
Agent has ACR etc..
Impact modifying agent is extremely important in PVC composite-material formula, is mainly used in improving the shock resistance of composite
Performance.The maximum shortcoming of PVC is too crisp, and shock resistance is poor, significantly limit PVC product in actual industrial
Application.The impact modifying agent commonly used at present is broadly divided into elastomeric material and rigid particles material.
It is commonly used auxiliary agent, the processing conditionss according to product and performance requirement in PVC composite-material formula above
Other auxiliary agents can be added, such as filler, coloring agent etc..
PVC resin can be according to actual need after adding heat stabilizer, lubricant, plasticizer etc. to improve processing characteristics
Other different auxiliary agent machine-shapings of interpolation are asked to prepare all kinds of various informative, different properties products.Under normal circumstances, PVC product
In process two classes are divided into according to the difference of blend auxiliary agent.
The first kind is to knead and pelletize dry-blend or pre-composition by double screw extruder, uses for machine-shaping.This
Apoplexy due to endogenous wind dry-blend is primarily referred to as the PVC dry state powder mixture of not plasticizer-containing or very small amount plasticizer, and it mainly exists
The forms such as high-speed mixer mix, and prepare hard PVC material；Pre-composition refers mainly to the compounding of the PVC containing plasticizer
Material, in high-speed mixer or kneader, mixing and swelling hygrometric state powder mixture, prepare flexible PVC material.Become
The type course of processing is as shown in Figure 1.
Equations of The Second Kind be by the formula materials containing a large amount of plasticizers in high-speed mixer or high speed dispersor mix homogeneously
Afterwards, obtain the paste material of stable performance, moderate viscosity after slurry grinding and deaeration.The machine-shaping process of PVC plastic paste
As shown in Figure 2.
For solving above-mentioned technical problem, the invention provides a kind of wallpaper PVC film, the preparation of described wallpaper PVC film
Method is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
The source chemicals of described PVC film include one or more of：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
Described wallpaper PVC film, is made up of the source chemicals of following weight portion：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
Described carbon fiber is PAN base carbon fibre, and described MgO nano-particle is cubic structure, and substantially spherical in shape, its particle diameter is
28-32nm.
Described wallpaper PVC film, can prepare expansion type PVC wallpaper further.
For solving above-mentioned technical problem, present invention also offers a kind of preparation method of wallpaper PVC film, step is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
The source chemicals of described PVC film include one or more of：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
The preparation of described wallpaper PVC film, is made up of the source chemicals of following weight portion：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
Described carbon fiber is PAN base carbon fibre, and described MgO nano-particle is cubic structure, and substantially spherical in shape, its particle diameter is
28-32nm.
For solving above-mentioned technical problem, invention further provides a kind of application of the preparation method of described wallpaper PVC film,
Described wallpaper PVC film, can be further used for preparing expansion type PVC wallpaper.
In PVC composite of the present invention, carbon fiber is filled in PVC composite, reaches PVC composite
Toughness reinforcing enhanced effect, adds metal oxide nanoparticles, reaches fire-retardant effect.
Prepare PVC composite of the present invention, composite production cost can be reduced.
Embodiment 1：The raw material of PVC film and equipment
1st, raw material（Following raw material is weight portion）
Material pvc（PVC）100 parts：SG-5, technical grade, Shaanxi North Yuan Chemical Group；
3 parts of carbon fiber, Zhejiang An Jie Industrial Equipment Co., Ltd.
Pb-Ba stabilizer 0.3：Foshan Han Bao auxiliary agent company limited；
1 part of paraffin：Shanghai Hua Shen rehabilitation material company limited；
2 parts of stearic acid：Shanghai Pu Shan Chemical Co., Ltd.；
Glycidyl methacrylate（GMA）2 parts：Tianjin Kermel Chemical Reagent Co., Ltd.；
Maleic anhydride（MAH）0.8 part：Tianjin Kermel Chemical Reagent Co., Ltd.；
Acrylic acid（AA）0.9 part：Tianjin Kermel Chemical Reagent Co., Ltd.；
Cumyl peroxide（DCP）0.5 part：Shanghai Ling Feng chemical reagent company limited；
Dual-tert-butyl peroxy isopropyl base benzene（BIPB）0.4 part：Hunan Yixiang Chemical Industrial Co., Ltd.；
Benzoyl peroxide（BPO）1 part：Tianjin good fortune morning chemical reagent factory；
Peroxidating di tert butyl carbonate（DTBP）0.8 part：Tianjin good fortune morning chemical reagent factory；
Styrene（St）2 parts：Chengdu Ke Long chemical reagent factory.
1.5 parts of epoxy resin E-44：Yueyang, hunan Ba Ling petrochemical industry company limited.
0.2 part of MgO nano-particle, self-control.
0.3 part of copper nanoparticle colloid solution, self-control.
2nd, equipment：
Opening rubber mixing machine：TY-160 type, Jiangdu high heaven and deep sea test machines factory；
Electric heating constant-temperature blowing drying box：DHG-9075A type, Shanghai Yiheng Scientific Instruments Co., Ltd；
High-speed mixer：SHR type, Ya Su Machinery Co., Ltd. of Zhangjagang City；
Parallel dual-screw extruding machine：SHJ-20 type, Nanjing Jie Ente electromechanics company limited；
Injection moulding machine：GEK-80 type, Zhejiang Jinying Plastic Machinery Co., Ltd.；
Micro-control electronic universal tester：WDW3020 type, Changchun Ke Xin experimental apparatus company limited；
Electron bombardment testing machine：XCJ-40 type, Chengde microtest machine company limited；
Static contact angle instrument：SL200B type, Ke Nuo Industrial Co., Ltd of the U.S.；
Scanning electron microscope（SEM）：TM3030 type, hitachi Hitachi, Ltd；
Optical microscope：N-180M type, Beijing Yongxin Norhua Science ＆ Technology Co., Ltd.；
Thermogravimetric analyzer（TGA）：STA-409PC type, Germany is resistance to speed.
Embodiment 2：Carbon fiber
Carbon fiber（Carbon fiber, abbreviation CF）, be a kind of high intensity more than 95% for phosphorus content, high modulus fibre new
Fiber type material.It is to be piled up along fiber axial direction by organic fibers such as flake graphite crystallites to form, through carbonization and graphitization
Micro crystal graphite material obtained from process.Carbon fiber " soft outside but hard inside ", quality is lighter than metallic aluminium, but intensity is higher than iron and steel, and
And there are corrosion-resistant, high-moduluss characteristics, it is all important materials in defence and military and civilian aspect.It not only has material with carbon element
Intrinsic intrinsic property, has both the soft machinability of textile fabric again, is reinforcing fiber of new generation.
Carbon fiber has many premium properties, and the axial strength of carbon fiber and modulus are high, and density is low, higher than performance, no compacted
Become, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, specific heat and electric conductivity between nonmetallic and metal between, thermal expansion system
Number is little and has anisotropy, good corrosion resistance, and X-ray transparent is good.Good electrical and thermal conductivity performance, electromagnetic wave shielding are good
Deng.
Compared with traditional glass fibre, Young's moduluss are them more than 3 times to carbon fiber；It compared with Kafra fiber, Young
Modulus is its 2 times about, insoluble not swollen in organic solvent, acid, alkali, and corrosion resistance projects.
Carbon fiber can be divided into polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose-based carbon fiber, phenolic aldehyde by raw material sources
Base carbon fibre, gas-phase growth of carbon fibre；Universal, high-strength, middle mold high-strength, high model and superelevation model can be divided into by performance
Carbon fiber；It is divided into long filament, chopped fiber and chopped strand by state；It is divided into universal and high-performance type by mechanical property.Universal
Carbon fiber strength is 1000 MPas, modulus is about 100G handkerchief.High-performance carbon fibers are divided into high-strength again（Intensity 2,000,000,000
Handkerchief, modulus 250G handkerchief）With high model（More than modulus 300G handkerchief）.Intensity be more than 4000 MPas be also called superelevation strong type；Modulus
Referred to as superelevation model more than 450G handkerchief.With the development of space flight and aircraft industry, have also appeared high-strength height and stretch type carbon fiber, its
Elongation percentage is more than 2%.What consumption was maximum is polyacrylonitrile (PAN) base carbon fibre.
The production technology of the PAN base carbon fibre that the present embodiment uses mainly includes precursor and produces and two mistakes of precursor carbonization
Journey:First pass through the series of process such as acrylonitrile polymerization and spinning be processed into and be referred to as " parent " and polyacrylonitrile fibre or former
Silk, these precursor is put in oxidation furnace and is aoxidized at 220 to 258 DEG C, also will arrive for 1300 in temperature in carbide furnace
Carry out carbonization and other processes at 1450 DEG C and make carbon fiber.
Embodiment 3：The present embodiment adopts indoor temperature solid phase method to prepare MgO granule.
Solid-phase reaction of the present invention overcomes the agglomeration traits that conventional wet prepares magnesium oxide nanoparticle presence, tool
Have the advantages that to react easy without solvent, yield height, reaction condition；And overcome efficiency present in original solid-phase reaction
The shortcoming of the oxidizable deformation of low, particle.
The concrete grammar that the present embodiment indoor temperature solid phase method prepares MgO granule is：By MgCI solution and Na2CO3（Raw materials quality
Proportioning 1:1.2）Solution, with PVA solution（Poly-vinyl alcohol solution）For modifying agent, reaction generation precipitation MgCO3Precipitation, then 75
Under ~ 85 DEG C of constant temperature, by way of precipitation converts, obtain alkali formula carbon formula magnesium presoma.Before 52 ~ 55 DEG C of standing alkali formula carbon formula magnesium
Drive body to precipitate 26 hours.Finally it is passed through in Ar air-flow, temperature is calcined under conditions of being 610 ~ 630 DEG C, has obtained nano-MgO
Grain.Using PVA as high molecular surfactant, control the reunion of granule, obtained nano-MgO particle dispersion is relatively
Good, it is cubic structure, substantially spherical in shape, its particle diameter is 28-32nm.
Embodiment 4：The preparation of copper nanoparticle colloid
Main agents：Sodium pyrophosphate（Solid, chemical reagent）, potassium borohydride（Solid, analytical reagent）, Polyvinylpyrrolidone
（PVP-K30, Mw=40000）, sodium potassium tartrate tetrahydrate（Solid, chemical reagent）, disodiumedetate（EDTA-2Na, solid, point
Analysis reagent）, copper sulfate（Solid, analytical reagent）, sodium hydroxide（Solid, chemical reagent）, sodium lauryl sulphate（SDS, Gu
Body, chemical reagent）, water is redistilled water.
Key instrument：ZHJ-2 timing motor stirrer, makes aerosol apparatus, ZK-82A type vacuum drying oven by oneself.
Copper-bath is prepared：Successively quantitative water, copper sulfate, EDTA-2Na, sodium potassium tartrate tetrahydrate and PVP are added taper
In bottle, stir；Then adjust pH value with sodium hydroxide to prepare to 13.3 solution of potassium borohydride：Successively by quantitative water, Jiao
Sodium phosphate and SDS add in conical flask, stir；With sodium hydroxide regulation pH value to 12；It is subsequently adding quantitative KBH4, stir
Mix uniformly；Finally with sodium hydroxide regulation pH value to 14.5.
The preparation process of Nanometer Copper：
Measure 8% copper-bath 500ml and 9% solution of potassium borohydride 600ml respectively；It is 33 DEG C and 8000KPS in temperature
Under high-speed stirred, with aerosol apparatus, copper-bath spray is added in the three-neck flask filling solution of potassium borohydride；Utilize acid simultaneously
The pH value of degree meter monitoring reactant liquor, and adds sodium hydroxide at any time, to keep the pH value of reactant liquor 14.5；After spray plus end,
Continue stirring, reaction about 8 minutes, reaction terminates.Product is the colloid solution of maroon. when preparing polyvinyl chloride resin, directly makes
Use this colloid solution.
Prepare after the TEM photo of colloid as can be seen that nanometer copper particle subglobular, basic soilless sticking, particle diameter is 8 ~
22nm, more than 80% particle diameter is 12 ~ 16nm.
Embodiment 5：The preparation of embodiment of the present invention wallpaper PVC film.
Each source chemicals aforementioned are proportionally added in high-speed mixer mixing 5min, obtain premix material.By double
Screw extruder melt extrudes, and becomes batten, and pulverizer is pulverized.Reuse the wall that injection moulding machine injection obtains the embodiment of the present invention
Paper PCV film.
Embodiment 6：PVC wallpaper of the present invention, can also be prepared as expansion type PVC wallpaper.PVC foam type wallpaper of the present invention,
Using the foaming that is rapidly heated.
The foaming that is rapidly heated is that a kind of application of supercritical fluid batch-foamed method is more widely prepared polymer and sent out
The process of foam material.Two stages are divided into based on the process substantially cocoa that the method for being rapidly heated prepares polymeric foamable material:
（1）Kettle pressure saturation stage and intensification foaming stages.Kettle presses the technological parameter of saturation stage to include：Saturation pressure, saturation temperature and
Saturation time, the technological parameter of intensification foaming stages includes blowing temperature and foamed time.Wherein, saturation pressure, saturation temperature,
Blowing temperature is three vital technological parameters of impact polymer foaming quality.
Prepare the foaming agent CO of poromerics2Purchased from Ningbo Kowloon gas Manufacturing Co., Ltd, purity is more than 99.5%.??
The saturating kettle of high pressure, HL150Lx2/25-SY type supercritical CO2Permeability apparatus, Hangzhou Hua Li Beng Ye company limited produces;
Water bath, self-control;
Electric heating (air blast) thermostatic drying chamber, 101A-1 type, Jiangsu Taizhou City Tian Tai electric heating instrument plant produces.
Foaming method used by the present invention is the foaming that is rapidly heated in batch-foamed method, and basic step is:First, will
Laboratory sample is put in high pressure permeability kettle and is sealed, and gas injection system is by high pressure CO2Gas is injected in kettle, so that pressure is reached
7.3MPaW is upper and adjusts golden temperature and reaches more than 31.2 DEG C, but needs, by temperature control below polymer Tg, to make kettle
Interior CO2Become supercriticality, through after a while, gradually form polymer/gas homogeneous saturation system.During one section of pressurize
Between after, unload rapidly and be depressed into normal pressure, polymer/SCCO2System enter hypersaturated state, formed thermodynamic unstable system, gather
Start cell nucleation inside compound, then quickly polymer samples put into heating a period of time in the water bath of design temperature,
On microcosmic, abscess continues nucleation and increases final curing sizing, and macroscopically polymer samples start significantly to foam and swell, and send out
Finish into.??
In the embodiment of the present invention, specific experiment parameter setting is as follows:??
(1) saturation pressure:The change of saturation pressure is set as 5MPa, 8 MPa, 11 MPa, 13MPa, 17 MPa, 20MPa.??
(2) saturation temperature:The change of saturation temperature is set as 27 DEG C, 30 DEG C, 33 DEG C, 36 DEG C, 38 DEG C, 42 DEG C.??
(3) saturation time:The change of saturation time is set as 1h, 2h, 3h, 4h, 5h, 6h.??
(4) blowing temperature:The change of blowing temperature is set as 75 DEG C, 83 DEG C, 88 DEG C, 90 DEG C, 95 DEG C, 100 DEG C.??
(5) foamed time:The change of foamed time is set as 4s, 7s, 10s, 13s, 16s, 19s.??
To three experiment parameters preparing poromerics, the cell diameter, cell density and the tensile strength that select sample are as sound
Should, the analysis carrying out two levels obtains the Optimal technique process of poromerics, test result indicate that:??
1) in the case of the condition identical such as saturation temperature, saturation time, blowing temperature, foamed time, the abscess of expanded material
Diameter is big gradually big with saturation pressure, and saturation pressure is excessive to occur serious cell collapse and coalescence phenomenon, sternly
Ghost image rings foaming quality.Temperature factor is to critical CO2The impact of molecular motion is very notable, with the liter of saturation temperature,
Foaming agent absorbtivity and escape amount alternately play mastery reaction, the increase of institute's saturation temperature, and the cell diameter of foaming sample is first
Plus after reduce.The impact to cell density for the blowing temperature is the most notable, and blowing temperature is higher, and the cell density of poromerics is got over
Greatly.??
2) present invention subsequently in orthogonal experiment using the saturation pressure of the embodiment of the present invention, saturation temperature and blowing temperature as
Factor of influence, as characterizing target, input is corresponding to characterize number for the cell diameter of foaming sample, cell density and tensile strength
According to, obtain transmission function, finally individual respond as considering, processing conditionss are optimized, have obtained PVC wallpaper supercritical of the present invention
CO2Prepare the Optimal technique process of polyvinyl-chloride foam material, that is, saturation pressure is 13MPa, saturation temperature is 38 DEG C, foaming temperature
Spend for 88 DEG C.Under above-mentioned process conditions, the cell diameter of the expanded material finally giving is 1.32 m, and cell density is
3.12*1010Individual/(cm3), tensile strength is 8.23MPa.??
Embodiment 7：Wallpaper of the present invention with the test of PVC film fire retardant performance and characterizes
Tested according to GB GB/T 2406-1993 according to the LOI of limited oxygen index (LOI) sample, concrete sample chi
Very little for long 70 × 6.5 × 3 (± 0.1) mm3, when sample burning times are less than 3min or burning length little 50mm, with oxygen volume
The critical concentration of the required nitrogen carrier of oxygen of fraction representation is the limited oxygen index of material.
Horizontal vertical burning grade (UL-94)
Carry out vertical combustion performance according to GB GB/T 2408-1996 to PP composite to test, sample size is
130×13×3mm3.Each sample of the present invention at least tests 5 samples, the combustibility of classified estimation recording materials.
Pure PVC after test material heats burning 30min in 400 DEG C of Muffle furnaces only has a small amount of black carbon residue residual,
And extravagance area is very big；PVC film sample of the present invention produces a loose greyish white carbon residue structure, and extravagant area is compared with pure PVC
Reduce；PVC foam wallpaper sample of the present invention produces a carbon residue structure relatively more compacting greyish white, and extravagant area is further
Reduce.
Mechanics Performance Testing
After PVC composite of the present invention placement at room temperature 3 days, (follow mark making 5B type dumbbell shaped batten with sampling machine
Quasi- GB/T 1,040 2006), Mechanics Performance Testing is done on universal testing machine with the speed of 200 mm/min.
Fire resistance is tested
After PVC composite of the present invention placement at room temperature 3 days, it is respectively cut into batten according to GB GB/T 2408.96,
Fire resistance test is done on Vertical combustion instrument.
Vertical combustion：UL.94 (plastics)
HB：Minimum flame retardant rating in UL94 standard.Require the sample for 3 to 13 millimeters thick, burning velocity is less than 40 millimeters
Per minute；Less than the sample of 3 millimeters thick, burning velocity is per minute less than 70 millimeters；Or extinguish before 100 millimeters of mark.
V_2：Sample is carried out twice after the combustion testing of 10 seconds, flame extinguished in 60 seconds.Comburant can be had to fall down.
V-1：Sample is carried out twice after the combustion testing of 10 seconds, flame extinguished in 60 seconds.Comburant can not be had to fall down.
V-0：Sample is carried out twice after the combustion testing of 10 seconds, flame extinguished in 30 seconds.Comburant can not be had to fall down.
Hot property
After PVC composite of the present invention placement at room temperature 3 days, take and thermal decomposition test is done in right amount on thermal analyzer（TG）,
Test condition is pure nitrogen gas, and heating rate is 20 degrees celsius/minute.And with pure PVC as reference.
In terms of the trend of the stress-strain diagram of the pure PVC without any process, stress is with the growth of Eva amount of tension
And increase.In the range of elongation 0-2cm, its stress has almost no change, and from the beginning of 2cm, its stress parabolically form
Increase.When elongation is for 14cm, reach stress maximum 140N.
Following table shows the impact to fracture tensile strength and elongation at break for the different experiments group（Matched group is pure PVC tree
Fat raw material；Experimental group 1-3 group is common PVC film of the present invention；Experimental group 4-6 is foaming PVC wallpaper of the present invention）：
| Experimental group | I | II | III | IV | V | VI | Matched group |
| Elongation at break % | 234.4 | 219.2 | 260.7 | 179.2 | 148.4 | 186.2 | 20.1 |
| Fracture tensile strength MPa | 15.4 | 14.7 | 13.7 | 13.6 | 12.7 | 12.5 | 10.3 |
Upper table shows the impact of the change to its elongation at break for different experiments group PVC.It will be apparent that each experimental group with pure
Fracture tensile strength between PVC matched group is obvious with elongation at break difference.
After PVC composite of the present invention placement at room temperature 3 days, it is respectively cut into according to GB GB/T 2408-96
150 × 150x3mm batten, does fire resistance test in Vertical combustion instrument, and result is as follows：
| Experimental group | Matched group | I | II | III | IV | V | VI |
| Average burning time first time（S） | 5 | 2 | 2 | 0 | 2 | 1 | 3 |
| Second average burning time（S） | 36（Molten drop） | 53 | 61 | 48 | 48 | 44 | 56 |
| Fire-retardant rank | No rank | V-2 | V-2 | V-2 | V-2 | V-2 | V-2 |
The above results illustrate the fire retardant cooperative flame retardant of six groups of experimental formulas of the present invention, can effectively improve flame retarding efficiency, reduce
Molten drop phenomenon when amount of flame-retardant agent and polymeric material burning；And the fire-retardant of fire proofing can be improved to a certain extent
Performance.
All above-mentioned this intellectual properties of primary enforcement, do not set this new product of enforcement limiting other forms
And/or new method.Those skilled in the art will be using this important information, and the above is changed, to realize similar execution feelings
Condition.But, all modifications or transformation belong to the right of reservation based on new product of the present invention.
Claims (10)
1. a kind of wallpaper PVC film is it is characterised in that the preparation method of described wallpaper PVC film is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
2. according to claim 1 wallpaper PVC film it is characterised in that the source chemicals of described PVC film include following one kind
Or it is multiple：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
3. according to claim 1 wallpaper PVC film it is characterised in that described wallpaper PVC film, by following weight portion
Source chemicals are made：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
4. according to claim 1 wallpaper PVC film it is characterised in that described carbon fiber is PAN base carbon fibre, described MgO
Nano-particle is cubic structure, substantially spherical in shape, and its particle diameter is 28-32nm.
5. wallpaper PVC film, it is characterised in that described wallpaper PVC film, can be prepared further according to claim 1
Expansion type PVC wallpaper.
6. a kind of preparation method of wallpaper PVC film is it is characterised in that step is：
Each source chemicals is proportionally added into mixing 5 ~ 8min in high-speed mixer, obtains premix material；
Melt extruded by double screw extruder, become batten, pulverizer is pulverized；
Reuse injection moulding machine injection and obtain described wallpaper PCV film.
7. according to claim 6 the preparation method of wallpaper PVC film it is characterised in that the source chemicals bag of described PVC film
Include one or more of：
Material pvc, carbon fiber, Pb-Ba stabilizer, paraffin, stearic acid, glycidyl methacrylate, maleic acid
Acid anhydride, acrylic acid, cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, peroxidating di tert butyl carbonate, benzene
Ethylene, epoxy resin E-44, MgO nano granule copper powder colloid.
8. according to claim 6 the preparation method of wallpaper PVC film it is characterised in that the system of described wallpaper PVC film
Standby, it is made up of the source chemicals of following weight portion：
100 parts of material pvc；
Carbon fiber 1-5 part；
Pb-Ba stabilizer 0.1-0.5；
Paraffin 0.5-2 part；
Stearic acid 1-3 part；
Glycidyl methacrylate 1-4 part；
Maleic anhydride 0.2-1.6 part；
Acrylic acid 0.4-1.3 part；
Cumyl peroxide 0.1-0.9 part；
Dual-tert-butyl peroxy isopropyl base benzene 0.2-0.6 part；
Benzoyl peroxide 0.5-2 part；
Peroxidating di tert butyl carbonate 0.3-1.2 part；
Styrene 1-3 part；
Epoxy resin E-44 1-3 part；
MgO nano-particle 0.1-0.4 part；
Copper nanoparticle colloid solution 0.1-0.4 part.
9. according to claim 6 wallpaper PVC film preparation method it is characterised in that described carbon fiber to be PAN base carbon fine
Dimension, described MgO nano-particle is cubic structure, substantially spherical in shape, and its particle diameter is 28-32nm.
10. a kind of application of the preparation method of wallpaper PVC film described in claim 6 is it is characterised in that described wallpaper PVC
Film, can be further used for preparing expansion type PVC wallpaper.
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| CN107142791A (en) * | 2017-05-06 | 2017-09-08 | 安徽玉发塑业有限公司 | A kind of anti-graffiti polyvinyl chloride wallpaper and preparation method thereof |
| CN107415271A (en) * | 2017-06-19 | 2017-12-01 | 江苏大海塑料股份有限公司 | A kind of production technology of anti-flammability PVC plastic Wallpaper film |
| CN109177014A (en) * | 2018-10-30 | 2019-01-11 | 海安亚鼎机电制造有限公司 | The processing method of staircase part |
| CN113510990A (en) * | 2020-09-29 | 2021-10-19 | 东莞市元普塑胶科技有限公司 | Artificial leather with artificial leather produced and prepared by supercritical nitrogen foaming technology |
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