CN109265720A - Hydrofluoric acid resistant nylon membrane and preparation method thereof - Google Patents
Hydrofluoric acid resistant nylon membrane and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
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- C08K7/00—Use of ingredients characterised by shape
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The invention discloses a kind of hydrofluoric acid resistant nylon membranes, according to parts by weight, including following component: 80-120 parts of nylon resin;5-15 parts of -2,5 di-t-butyl hexane peroxide of 2,5- dimethyl;10-20 parts of carbon fiber;TiO2/ it is modified ZrO230-40 parts of composite material;20-33 parts of glass fibre;5-10 parts of dispersing agent.Being uniformly distributed for carbon fiber and glass fibre is realized by dispersing agent, promotes whole acid resistance, avoids part from excessively concentrating, furthermore with the high-performance of cheap and the carbon fiber of glass fibre, coordination is reached in mixing ratio, plays the purpose for controlling cost.In addition the present invention utilizes 2,5- dimethyl -2,5 di-t-butyl hexane peroxide, allows entirety that reticular structure is presented, and utilize TiO2/ it is modified ZrO2Composite material enhances whole Antacid effectiveness.
Description
Technical field
The present invention relates to nylon membrane, in particular to a kind of hydrofluoric acid resistant nylon membrane and preparation method thereof.
Background technique
The application for a patent for invention of one Patent No. CN1340444A discloses a kind of soft package structure of battery core and its manufacture
Method.It is packed using the excellent plastic-aluminum packaging film of water proof, air-tightness, by its one side doubling, another three sides difference order into
Row heating plastic packaging.Battery is encapsulated in plastic-aluminum packaging film by this specific heat-sealing order.
Do not have to record the structure and its manufacturing method of plastic-aluminum packaging film in the invention patent application, as far as the applicant is aware, this
Plastic-aluminum packaging film is food, drug heat sealed package film;But food and Key works Drug packing film do not have anti-flexible packing lithium ion battery and
The function of polymer lithium ion battery electric solution liquid and hydrofluoric acid corrosion, also not having punch forming is box-packed performance.Actually
Existing plastic-aluminum packaging film is all food, drug heat sealed package film, cannot function as lithium ion battery packaging film use, i.e., enabled
Enough using effects are also undesirable, and anti-corrosion capability is weak, has much room for improvement.
Summary of the invention
The object of the present invention is to provide a kind of hydrofluoric acid resistant nylon membranes, have the advantages that hydrofluoric acid resistant.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of hydrofluoric acid resistant nylon membrane, according to parts by weight, including following component:
80-120 parts of nylon resin;
2,5- 5-15 parts of dimethyl -2,5 di-t-butyl hexane peroxides;
10-20 parts of carbon fiber;
TiO2/ it is modified ZrO230-40 parts of composite material;
20-33 parts of glass fibre;
5-10 parts of dispersing agent.
By using above-mentioned technical proposal, being uniformly distributed for carbon fiber and glass fibre is realized by dispersing agent, is promoted whole
The acid resistance of body avoids part from excessively concentrating, furthermore with the high-performance of the cheap and carbon fiber of glass fibre, in match ratio
Reach coordination in example, plays the purpose of control cost.In addition the present invention using 2,5- dimethyl -2,5 di-tert-butyl peroxide oneself
Alkane allows entirety that reticular structure is presented, and utilizes TiO2/ it is modified ZrO2Composite material enhances whole Antacid effectiveness.
The present invention is further arranged to: further including having isopropyl three (dioctylphyrophosphoric acid acyloxy) titanium according to parts by weight
5-10 parts of acid esters.
By using above-mentioned technical proposal, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters can be improved TiO2/
Modified ZrO2The adhesive force and covering power of composite material play the performance for enhancing whole hydrofluoric acid resistant.
The present invention is further arranged to: the modified ZrO2Method of modifying, to ZrO under conditions of 300-400 DEG C2Into
Row calcining is until ZrO2Crystal structure be in tetragonal phase.
By using above-mentioned technical proposal, the ZrO of tetragonal phase state2Corrosion resistance it is most strong relative to other crystal.
The present invention is further arranged to: the TiO2/ it is modified ZrO2The preparation method of composite material:
Compare according to parts by weight, TiO2/ it is modified ZrO2In 30-40 parts of composite material, by TiO2: modified ZrO2=1: 3 mixing, and
It is added 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy), continues 3 hours under conditions of 80 DEG C.
Three (dioctylphyrophosphoric acid of isopropyl can be easily obtained using above scheme by using above-mentioned technical proposal
Acyloxy) titanate esters.
The present invention is further arranged to: dispersing agent chooses vinyl bis-stearamides.
The present invention is further arranged to: according to parts by weight, 2,5- dimethyl -2,5 di-tert-butyl peroxide oneself
8 parts of methacrylic acid are added in 5-15 parts of alkane, and under conditions of 100 DEG C, continues 3h.
Methacrylic acid is allowed to be grafted on 2,5- dimethyl-by the way that methacrylic acid is added by using above-mentioned technical proposal
In 2,5 di-t-butyl hexane peroxides, enhance the steric hindrance of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide.
It is a further object to provide a kind of preparation methods of hydrofluoric acid resistant nylon membrane, include the following steps:
Step 1: according to parts by weight, after weighing 10-20 parts and glass fibre 20-33 parts mixing of carbon fiber, under conditions of 50 DEG C
5-10 parts of titanate esters of addition isopropyl three (dioctylphyrophosphoric acid acyloxy);
Step 2: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase, changed
Property ZrO2;
Step 3: comparing according to parts by weight, weigh TiO2/ZrO230-40 parts of composite material, wherein pressing TiO2: modified ZrO2=1: 3
Mixing, and 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy) is added, continue 3 hours under conditions of 80 DEG C;
Step 4: according to parts by weight, methyl is added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide
8 parts of acrylic acid, and under conditions of 100 DEG C, continue 3h;
Step 5: by product mix that step 1, step 2, step 3 and step 4 obtain and 80-120 parts of nylon resin and second is added
5-10 parts of alkenyl bis-stearamides obtain finished product;
Step 6: according to parts by weight, fluorine gas being sprayed to the surface of finished product.
By using above-mentioned technical proposal, the present invention is allowed easily to prepare hydrofluoric acid resistant nylon membrane.
In conclusion the invention has the following advantages:
1, the present invention is handled the outer surface of nylon membrane using the fluorine gas of strong oxidizing property, and fine and close fluorination is formed in outer surface
Nitride layer is able to bear the corrosion of hydrofluoric acid since the stability of fluoride is stronger.
2, under the action of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide, nylon resin will constitute intertexture net
Shape, the greatly whole intensity of enhancing, and after 2,5- dimethyl -2,5 di-t-butyl hexane peroxide grafted methacrylic acid, by
In the addition of methacrylic acid, steric hindrance increases, and reduces contact of the extraneous hydrofluoric acid with nylon resin, and then slow down reaction speed
Rate.
3, under conditions of 400 DEG C, to ZrO2It is calcined, until ZrO2At tetragonal phase structure, ZrO2Tetragonal phase structure mentions
High whole acid-alkali-corrosive-resisting performance, and ZrO2The pairs of acid-alkali-corrosive-resisting performance of crystal form group is affected.
Detailed description of the invention
Fig. 1 is ZrO2Tetragonal body structural schematic diagram.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
Embodiment 1:
A kind of hydrofluoric acid resistant nylon membrane, according to parts by weight, including following component:
80-120 parts of nylon resin, modified 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide, carbon fiber 10-20
Part, TiO2/ it is modified ZrO210-20 parts of composite material, 20-33 parts of glass fibre, 5-10 parts of vinyl bis-stearamides, isopropyl
Three 5-10 parts of titanate esters of (dioctylphyrophosphoric acid acyloxy).
Above-mentioned modified ZrO2Preparation method: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal
Structure is in tetragonal phase.
Above-mentioned TiO2/ it is modified ZrO2The preparation method of composite material: compare according to parts by weight, TiO2/ it is modified ZrO2Composite wood
In 30-40 parts of material, by TiO2: modified ZrO2=1: 3 mixing, and isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters are added
5-10 parts, continue 3 hours under conditions of 80 DEG C.
Above-mentioned modification 2, the preparation method of 5-15 parts of 5- dimethyl -2,5 di-t-butyl hexane peroxide:
According to parts by weight, 8 parts of methacrylic acid are added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide,
And under conditions of 100 DEG C, continue 3h.
A kind of preparation method of hydrofluoric acid resistant nylon membrane, includes the following steps:
Step 1: according to parts by weight, after weighing 10-20 parts and glass fibre 20-33 parts mixing of carbon fiber, under conditions of 50 DEG C
5-10 parts of titanate esters of addition isopropyl three (dioctylphyrophosphoric acid acyloxy);
Step 2: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase, changed
Property ZrO2;
Step 3: comparing according to parts by weight, weigh TiO2/Zr0230-40 parts of composite material, wherein pressing TiO2: modified ZrO2=1: 3
Mixing, and 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy) is added, continue 3 hours under conditions of 80 DEG C;
Step 4: according to parts by weight, metering system is added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide
8 parts of acid, and under conditions of 100 DEG C, continue 3h;
Step 5: by product mix that step 1, step 2, step 3 and step 4 obtain and 80-120 parts of nylon resin and second is added
5-10 parts of alkenyl bis-stearamides;
Step 6: according to parts by weight, fluorine gas being sprayed to the surface of finished product.
(dioctylphyrophosphoric acid acyloxy) titanate coupling agent of isopropyl three is adopted to Longgang District of Shenzhen City Ding Guo plastic cement firm
Filler can be improved in coating to treatment inorganic filling material significant effect in purchase, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three
In dispersion and bonding, improve processing fluidity, improve the mechanical strength of coating.
Above-mentioned nylon resin is bought to Guangzhou Xin Sheng engineering plastics Co., Ltd.
Above-mentioned carbon fiber is bought to Fu Desen carbon fiber Science and Technology Ltd..
Above-mentioned isopropyl three (dioctylphyrophosphoric acid acyloxy) is bought to Zhejiang boiling point Chemical Co., Ltd..
It is proved through practical application, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters can be improved TiO2/ it is modified ZrO2
The adhesive force and covering power of composite material play the performance for enhancing whole hydrofluoric acid resistant.
Embodiment 2:
It is with the distinctive points of embodiment 1, a kind of hydrofluoric acid resistant nylon membrane, according to parts by weight, including following component:
80-120 parts of nylon resin, modified 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide, carbon fiber 10-20
Part, TiO2/ it is modified ZrO210-20 parts of composite material, 20-33 parts of glass fibre, 5-10 parts of vinyl bis-stearamides, isopropyl
Three 5-10 parts of titanate esters of (dioctylphyrophosphoric acid acyloxy).
Above-mentioned modified ZrO2Preparation method: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal
Structure is in tetragonal phase.
Above-mentioned TiO2/ it is modified ZrO2The preparation method of composite material: compare according to parts by weight, TiO2/ it is modified ZrO2Composite wood
In 30-40 parts of material, by TiO2: modified ZrO2=1: 3 mixing, and isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters are added
5-10 parts, continue 3 hours under conditions of 80 DEG C.
Above-mentioned modification 2, the preparation method of 5-15 parts of 5- dimethyl -2,5 di-t-butyl hexane peroxide:
According to parts by weight, 8 parts of methacrylic acid are added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide,
And under conditions of 100 DEG C, continue 3h.
A kind of preparation method of hydrofluoric acid resistant nylon membrane, includes the following steps:
Step 1: according to parts by weight, after weighing 10-20 parts and glass fibre 20-33 parts mixing of carbon fiber, under conditions of 50 DEG C
5-10 parts of titanate esters of addition isopropyl three (dioctylphyrophosphoric acid acyloxy);
Step 2: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase, changed
Property ZrO2;
Step 3: comparing according to parts by weight, weigh TiO2/ZrO230-40 parts of composite material, wherein pressing TiO2: modified ZrO2=1: 3
Mixing, and 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy) is added, continue 3 hours under conditions of 80 DEG C;
Step 4: according to parts by weight, metering system is added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide
8 parts of acid, and under conditions of 100 DEG C, continue 3h;
Step 5: by product mix that step 1, step 2, step 3 and step 4 obtain and 80-120 parts of nylon resin and second is added
5-10 parts of alkenyl bis-stearamides;
Step 6: according to parts by weight, fluorine gas being sprayed to the surface of finished product.
Embodiment 3:
It is with the distinctive points of embodiment 1, a kind of hydrofluoric acid resistant nylon membrane, according to parts by weight, including following component:
80-120 parts of nylon resin, modified 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide, carbon fiber 10-20
Part, TiO2/ it is modified ZrO210-20 parts of composite material, 20-33 parts of glass fibre, 5-10 parts of vinyl bis-stearamides, isopropyl
Three 5-10 parts of titanate esters of (dioctylphyrophosphoric acid acyloxy).
Above-mentioned modified ZrO2Preparation method: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal
Structure is in tetragonal phase.
Above-mentioned TiO2/ it is modified ZrO2The preparation method of composite material: compare according to parts by weight, TiO2/ it is modified ZrO2Composite wood
In 30-40 parts of material, by TiO2: modified ZrO2=1: 3 mixing, and isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters are added
5-10 parts, continue 3 hours under conditions of 80 DEG C.
Above-mentioned modification 2, the preparation method of 5-15 parts of 5- dimethyl -2,5 di-t-butyl hexane peroxide:
According to parts by weight, 8 parts of methacrylic acid are added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide,
And under conditions of 100 DEG C, continue 3h.
A kind of preparation method of hydrofluoric acid resistant nylon membrane, includes the following steps:
Step 1: according to parts by weight, after weighing 10-20 parts and glass fibre 20-33 parts mixing of carbon fiber, under conditions of 50 DEG C
5-10 parts of titanate esters of addition isopropyl three (dioctylphyrophosphoric acid acyloxy);
Step 2: to Zr0 under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase, changed
Property ZrO2;
Step 3: comparing according to parts by weight, weigh TiO2/ZrO230-40 parts of composite material, wherein pressing TiO2: modified ZrO2=1: 3
Mixing, and 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy) is added, continue 3 hours under conditions of 80 DEG C;
Step 4: according to parts by weight, metering system is added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide
8 parts of acid, and under conditions of 100 DEG C, continue 3h;
Step 5: by product mix that step 1, step 2, step 3 and step 4 obtain and 80-120 parts of nylon resin and second is added
5-10 parts of alkenyl bis-stearamides;
Step 6: according to parts by weight, fluorine gas being sprayed to the surface of finished product.
Comparative example 1: being with the distinctive points of embodiment 2, and the surface sprinkling fluorine gas to finished product is eliminated in preparation method
Step.
Comparative example 2: being with the distinctive points of embodiment 2, not to progress ZrO2It is calcined.
Test experiments weigh embodiment 1, embodiment 2, embodiment 3, comparative example 1 and comparison according to identical parts by weight
Example 2.It allows embodiment 1, embodiment 2, embodiment 3, comparative example 1 and comparative example 2 to impregnate 85 DEG C, 7 days in the electrolytic solution, measures film layer
Between peel strength.
Table 1 is the performance table of embodiment 1, embodiment 2, embodiment 3, comparative example 1 and comparative example 2.
Comparative example 3: being with the distinctive points of embodiment 2, not to 2,5- dimethyl -2,5 di-t-butyl hexane peroxide into
Row is modified.
Table 2 is the performance table of embodiment 1, embodiment 2, embodiment 3, comparative example 3.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (7)
1. a kind of hydrofluoric acid resistant nylon membrane, it is characterized in that: according to parts by weight, including following component:
80-120 parts of nylon resin;
5-15 parts of -2,5 di-t-butyl hexane peroxide of 2,5- dimethyl;
10-20 parts of carbon fiber;
TiO2/ it is modified ZrO230-40 parts of composite material;
20-33 parts of glass fibre;
5-10 parts of dispersing agent.
2. hydrofluoric acid resistant nylon membrane according to claim 1, it is characterized in that: further including having isopropyl three according to parts by weight
5-10 parts of titanate esters of (dioctylphyrophosphoric acid acyloxy).
3. hydrofluoric acid resistant nylon membrane according to claim 1, it is characterized in that: the modified ZrO2Method of modifying, in 300-
To ZrO under conditions of 400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase.
4. hydrofluoric acid resistant nylon membrane according to claim 3, it is characterized in that: the TiO2/ it is modified ZrO2The system of composite material
Preparation Method:
Compare according to parts by weight, TiO2/ it is modified ZrO2In 30-40 parts of composite material, by TiO2: modified ZrO2=1:3 mixing, and add
Enter 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy), continues 3 hours under conditions of 80 DEG C.
5. hydrofluoric acid resistant nylon membrane according to claim 1, it is characterized in that: dispersing agent chooses vinyl bis-stearamides.
6. hydrofluoric acid resistant nylon membrane according to claim 1, it is characterized in that: according to parts by weight, in 2, the 5- diformazan
8 parts of methacrylic acid are added in 5-15 parts of base -2,5 di-t-butyl hexane peroxide, and under conditions of 100 DEG C, continues
3h。
7. the preparation method of hydrofluoric acid resistant nylon membrane described in -6 according to claim 1, it is characterized in that: including the following steps:
Step 1: according to parts by weight, after weighing 10-20 parts and glass fibre 20-33 parts mixing of carbon fiber, under conditions of 50 DEG C
5-10 parts of titanate esters of addition isopropyl three (dioctylphyrophosphoric acid acyloxy);
Step 2: to ZrO under conditions of 300-400 DEG C2Calcining is carried out until ZrO2Crystal structure be in tetragonal phase, be modified
ZrO2;
Step 3: comparing according to parts by weight, weigh TiO2/ZrO230-40 parts of composite material, wherein pressing TiO2: modified ZrO2=1:3
Mixing, and 5-10 parts of titanate esters of isopropyl three (dioctylphyrophosphoric acid acyloxy) is added, continue 3 hours under conditions of 80 DEG C;
Step 4: according to parts by weight, first is added in 5-15 parts of 2,5- dimethyl -2,5 di-t-butyl hexane peroxide
8 parts of base acrylic acid, and under conditions of 100 DEG C, continue 3h;
Step 5: by product mix that step 1, step 2, step 3 and step 4 obtain and 80-120 parts of nylon resin and second is added
5-10 parts of alkenyl bis-stearamides obtain finished product;
Step 6: according to parts by weight, fluorine gas being sprayed to the surface of finished product.
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