CN108486881A - A kind of preparation method of collagen/PA superfine fibre non-woven materials - Google Patents
A kind of preparation method of collagen/PA superfine fibre non-woven materials Download PDFInfo
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- CN108486881A CN108486881A CN201810230380.6A CN201810230380A CN108486881A CN 108486881 A CN108486881 A CN 108486881A CN 201810230380 A CN201810230380 A CN 201810230380A CN 108486881 A CN108486881 A CN 108486881A
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- ldpe
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
Abstract
The invention discloses a kind of preparation methods of collagen/PA superfine fibre non-woven materials, are specifically implemented according to the following steps：Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and obtains CMA PA/LDPE non-woven materials；Step 3, CMA PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials.The method of the present invention impregnates membrane formation process with green technological process collagen and replaces the how heavy-polluted polyurethane impregnated technique of original consumption of organic solvent, it can be effectively improved a large amount of solvent contamination phenomenon that current solvent borne polyurethane impregnation technology is brought, mitigate environmental pollution significantly.
Description
Technical field
The invention belongs to high molecular material and function textile material technical fields, and in particular to a kind of collagen/PA is super
The preparation method of fine fibre non-woven material.
Background technology
Superfine fiber chemical leather base material is the superfine fibre to be interweaved by three-dimensional and the filling polyurethane body with microcellular structure
The composite material being combined, 4 key links of manufacture, which include superfine fibre manufacture, density three-dimensional is solid netted non-knits
Make cloth manufacture, the manufacture of open type microcellular structure polyurethane film and surface layer manufacturing technology.By this technology, make superfine fiber chemical leather
Natural leather can be simulated in terms of appearance, function, perception.The structure that collagenous fibril is simulated with superfine fibre, uses fiber
Three-D non-woven structural simulation natural leather in collagenous fibres weave form, make superfine fiber chemical leather from microstructure, outer
Texture, physical characteristic etc. are seen, all achievees the effect that emulation.
Superfine fiber chemical leather manufacture is divided into figured type and non-figured type according to its spining technology to classify, as shown in Figure 1.
Figured type technology is that " sea " component is melted by individual screw extruder respectively with " island " component, then arrive filament spinning component into
Row is compound.It is not detached between island during spinning technique, keeps monofilament form.Meanwhile island component is not glued in forming process
Even (good between monofilament lagoon island and island to detach) island component is that continuous uniform is distributed on the length direction of fiber, and island number is solid
Fixed and fiber number is consistent, generally can only achieve 0.1~0.5dtex or so.It is to exist with conventional fiber number after composite spinning, only will
" sea " ingredient dissolves, and just can really obtain superfine fibre.The islands Fei Ding technology is made by incompatible polymer co-blended spinning,
It is also to exist with conventional fiber number after spinning.From determine unlike the fiber of island, the size, quantity on island, distribution in indefinite island fiber
And its all there is randomness in length in a certain range.There are many quantity on island, so average linear density smaller, with solvent extraction sea
After component fiber be in pencil, single fiber fiber number generally in 0.01~0.00ldtex or so, even up to 0.0001dtex, thus with
Collagenous fibres are more like.Therefore, superfine fiber chemical leather base material be exactly after decrement do not carry out make face, raising, dyeing
The synthetic leather semi-finished product of equal final finishings.The chief component of superfine fiber chemical leather product is exactly superfine fiber chemical leather base
Material is equivalent to the crust leather of corium.Therefore, the size of the moisture absorption water vapour permeability of base material directly determines superfine fiber chemical leather end
Hold the quality of the sanitation performance of product.
In recent years, Chinese synthetic leather industrial development is rapid, and there is a sharp increase in output, Market competition, and leather goods industry is to synthesis
The performance requirement for removing from office material is more and more high, the inexorable trend that develops into the field of the synthetic leather to emulational leather direction.It is ultra-fine
Fiber synthetic leather belongs to high-grade emulation skin product, it has the characteristics and advantages of many natural leathers, in mechanical strength, chemical resistance
Energy, mass uniformity and automation cut out flexibility (adaptability) of operation etc. and are better than natural leather.But compared with natural leather, inhale
Drenched wet performance has a long way to go, and dress is sultry, so its moisture absorption water vapour permeability urgently improves.
Currently, the research for Fypro surface modifying method in superfine fiber chemical leather base material has very much, such as table
Face absorption method, surface etch chemistry method, coupling agent modified technology etc..Most of the reacting due to Fypro of these methods
Active site is very little, and reaction efficiency is low, causes the hydrophilic radical that can subsequently introduce fiber surface limited, to also limit base
The raising of material moisture absorption water vapour permeability.Therefore for require to have efficiently, for functional stabilization, these features for being firmly combined with,
Such method is also difficult to meet these requirements.
Invention content
The object of the present invention is to provide a kind of preparation methods of collagen/PA superfine fibre non-woven materials, solve
By traditional polyurethane impregnated process bands Lai DMF pollution problems, also by control microstructure obtain highly hygroscopic penetrability work(
The comfort type synthetic leather composite material of the superfine fibre enhancing of energy.
The technical solution adopted in the present invention is a kind of preparation method of collagen/PA superfine fibre non-woven materials,
It is specifically implemented according to the following steps：
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials.
It is of the invention to be further characterized in that,
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 13%~83% vinyl collagen to take degree of substitution, and then addition ultraviolet light draws thereto
It sends out agent to be uniformly mixed, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:100~7:50, and concussion dispersion 30min~60min in supersonic wave cleaning machine, obtain the PA/ for being soaked with collagen
LDPE non-woven material samples.
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 3h~6h, obtains CMA-PA/LDPE non-woven materials.
The specific implementation process of step 3 is：It is 70 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C~90 DEG C of toluene in, carry out decrement treatment using small model machine, processing time is 90min~120min, will after decrement
Treated, and CMA-PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, are set again later
Ultrasonic washing is carried out in 50 DEG C of water, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and water is controlled, and low temperature is dry
It is dry, both obtain collagen/PA materials.
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm.
In step 1.2, the solid content of CMA solution is 6% ± 0.5%.
The invention has the advantages that
(1) collagen is introduced into the island superfine fiber non-woven material system not being reduced by the method for the present invention, is made
It makes the low density polyethylene olefinic constituent in two components using decrement in the surface-crosslinked film forming of two components (PA/LDPE) fiber
Dissolve away, to obtain highly hygroscopic penetrability two-phase inierpeneirating network structure non-woven material (the non-woven materials of CMA-PA/LDPEE
Material), traditional PU films are replaced with collagen film, finally obtain two-phase (PA-CMA) inierpeneirating network structure of highly hygroscopic penetrability
Superfine fibre non-woven material (collagen/PA materials)；
(2) the method for the present invention replaces original consumption of organic solvent more with green technological process collagen dipping membrane formation process
Heavy-polluted polyurethane impregnated technique can be effectively improved a large amount of solvent contamination that current solvent borne polyurethane impregnation technology is brought
Phenomenon mitigates environmental pollution significantly.
Description of the drawings
Fig. 1 is the traditional processing technology flow chart of superfine fiber chemical leather base material；
Fig. 2 is the process flow chart of the method for the present invention.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of collagen/PA superfine fibre non-woven materials of the present invention, shown in 1-2 as shown in the figure,
The preparation process of middle PA/LEPE non-woven materials uses the Conventional processing methods of superfine fiber chemical leather base material, work of the invention
Process is specifically implemented according to the following steps to later process route, the present invention since PA/LEPE non-woven materials：
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 13%~83% vinyl collagen to take degree of substitution, and then addition ultraviolet light draws thereto
It sends out agent to be uniformly mixed, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6% ± 0.5%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:100~7:50, and concussion dispersion 30min~60min in supersonic wave cleaning machine, obtain the PA/ for being soaked with collagen
LDPE non-woven material samples；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 3h~6h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 70 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C~90 DEG C of toluene in, carry out decrement treatment using small model machine, processing time is 90min~120min, will after decrement
Treated, and CMA-PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, are set again later
Ultrasonic washing is carried out in 50 DEG C of water, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and water is controlled, and low temperature is dry
It is dry, both obtain collagen/PA materials.
The present invention will be described in terms of principle below：
In step 1, vinyl collagen (CMA) solution impregnates PA/LDPE non-woven materials；
(a) it pre-processes
Ensure PA/LDPE in subsequent treatment process not because impurity there are due to influence technological effect, this step is mainly
Understand impurity, and makes have certain water content in PA/LDPE materials.
(b) vinyl collagen (CMA) solution impregnates PA/LDPE non-woven materials
The target of this step key is that vinyl collagen solution is enable uniformly adequately to infiltrate through entire PA/LDPE
In nonwoven substrates, so carrying out ultrasonic disperse using ultrasonic wave, jitter time about controls 30min~60min.In addition, adopting
It just can guarantee smoothly completing for the self-crosslinking film-forming process of next step with the vinyl collagen with certain degree of substitution.
In step 2, vinyl collagen (CMA) self-crosslinking in PA/LDPE non-woven materials forms a film：
The cardinal principle of this step vinyl collagen self-crosslinking film forming is free radical polymerization addition reaction, and chemistry is anti-
Answer principle as follows：
(1) chain causes
(2) chain growth
(3) chain termination
In step 3, the decrement extraction of CMA-PA/LDPE materials：
Decrement extraction principle can be dissolved in this characteristic in hot toluene using polyethylene, using hot toluene as polyethylene
Extractant makes the CMA-PA/LDPE materials of gained in step 2 in a large amount of hot toluenes, and through impregnating repeatedly, squeezing liquid with pressure roller makes
LDPE and various additives in composite fibre are extracted removing, to make fiber be in pencil hyperfine structure.
Embodiment 1
A kind of preparation method of collagen/PA superfine fibre non-woven materials, is specifically implemented according to the following steps：
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 13% vinyl collagen to take degree of substitution, and then addition ultraviolet initiator is mixed thereto
It closes uniformly, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:100, and the concussion dispersion 30min in supersonic wave cleaning machine, obtain the PA/LDPE non-woven materials for being soaked with collagen
Sample；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 3h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 70 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time 90min will treated CMA- after decrement
PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, place it in again later in 50 DEG C of water into
Row ultrasound washing, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and controls water, and low temperature drying both obtains collagen egg
In vain/PA materials.
Embodiment 2
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 50% vinyl collagen to take degree of substitution, and then addition ultraviolet initiator is mixed thereto
It closes uniformly, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6.25%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:80, and the concussion dispersion 40min in supersonic wave cleaning machine, obtain the PA/LDPE non-woven materials for being soaked with collagen
Sample；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 4h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 80 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time 100min will treated CMA- after decrement
PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, place it in again later in 50 DEG C of water into
Row ultrasound washing, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and controls water, and low temperature drying both obtains collagen egg
In vain/PA materials.
Embodiment 3
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 83% vinyl collagen to take degree of substitution, and then addition ultraviolet initiator is mixed thereto
It closes uniformly, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6.5%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:70, and the concussion dispersion 50min in supersonic wave cleaning machine, obtain the PA/LDPE non-woven materials for being soaked with collagen
Sample；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 5h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 85 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time 110min will treated CMA- after decrement
PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, place it in again later in 50 DEG C of water into
Row ultrasound washing, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and controls water, and low temperature drying both obtains collagen egg
In vain/PA materials.
Embodiment 4
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 70% vinyl collagen to take degree of substitution, and then addition ultraviolet initiator is mixed thereto
It closes uniformly, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:60, and the concussion dispersion 60min in supersonic wave cleaning machine, obtain the PA/LDPE non-woven materials for being soaked with collagen
Sample；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 6h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 90 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time 115min will treated CMA- after decrement
PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, place it in again later in 50 DEG C of water into
Row ultrasound washing, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and controls water, and low temperature drying both obtains collagen egg
In vain/PA materials.
Embodiment 5
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40
Ultrasound washing 30min in DEG C hot water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity,
Then naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 83% vinyl collagen to take degree of substitution, and then addition ultraviolet initiator is mixed thereto
It closes uniformly, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
In step 1.2, the solid content of CMA solution is 6.5%；
Step 1.3, it is mixed with what the pretreated PA/LDPE non-woven material samples of step 1.1 were put into that step 1.2 obtains
In the vinyl collagen solution of ultraviolet initiator, and the quality of PA/LDPE non-woven materials and vinyl collagen
Than being 7:50, and the concussion dispersion 60min in supersonic wave cleaning machine, obtain the PA/LDPE non-woven materials for being soaked with collagen
Sample；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-to obtain CMA-PA/LDPE
Weaving material；
The specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/ for being soaked with collagen is taken out
LDPE samples, directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination,
Naturally dry is taken out after irradiation 6h, obtains CMA-PA/LDPE non-woven materials；
In step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm,
Irradiation distance 15cm；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials；
The specific implementation process of step 3 is：It is 75 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time 120min will treated CMA- after decrement
PA/LDPE non-woven materials are submerged into DMF solvent, are cleaned by ultrasonic about 30min, place it in again later in 50 DEG C of water into
Row ultrasound washing, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and controls water, and low temperature drying both obtains collagen egg
In vain/PA materials.
Claims (6)
1. a kind of preparation method of collagen/PA superfine fibre non-woven materials, which is characterized in that specifically according to the following steps
Implement：
Step 1, PA/LDPE non-woven materials are impregnated using vinyl collagen solution；
Step 2, vinyl collagen self-crosslinking in PA/LDPE non-woven materials forms a film, and it is non-woven to obtain CMA-PA/LDPE
Material；
Step 3, CMA-PA/LDPE non-woven materials are reduced and are extracted out, obtain collagen/PA materials.
2. a kind of preparation method of collagen according to claim 1/PA superfine fibre non-woven materials, feature exist
In step 1 is specifically implemented according to the following steps：
Step 1.1, the pretreatment of PA/LDPE non-woven materials
PA/LDPE non-woven materials are cut into several PA/LDPE disks with the disk sampler of a diameter of 55cm, in 40 DEG C of heat
Ultrasound washing 30min in water, pressure rolling, pressure 1.5Mpa are taken out per 10min, and continuous washing pressure rolling 3 times washes away impurity, then
Naturally dry is weighed；
Step 1.2, PA/LDPE non-woven materials are impregnated using vinyl collagen solution
It is the CMA solution of 13%~83% vinyl collagen to take degree of substitution, then adds ultraviolet initiator thereto
It is uniformly mixed, mass concentration of the ultraviolet initiator in CMA solution is 0.0025%；
Step 1.3, the pretreated PA/LDPE non-woven material samples of step 1.1 being mixed with of being put into that step 1.2 obtains is ultraviolet
In the vinyl collagen solution of photoinitiator, and PA/LDPE non-woven materials and the mass ratio of vinyl collagen are
7:100~7:50, and concussion dispersion 30min~60min in supersonic wave cleaning machine, obtain the PA/LDPE for being soaked with collagen
Non-woven material sample.
3. a kind of preparation method of collagen according to claim 2/PA superfine fibre non-woven materials, feature exist
In the specific implementation process of step 2 is：After the completion of waiting for step 1.2 concussion dispersion, the PA/LDPE examinations for being soaked with collagen are taken out
Sample is directly put it on polyfluortetraethylene plate, then polyfluortetraethylene plate is placed in UV crosslinking instrument and carries out illumination, irradiates 3h
Naturally dry is taken out after~6h, obtains CMA-PA/LDPE non-woven materials.
4. a kind of preparation method of collagen according to claim 1/PA superfine fibre non-woven materials, feature exist
In the specific implementation process of step 3 is：It is 70 DEG C~90 that the CMA-PA/LDPE non-woven materials that step 2 obtains, which are placed in temperature,
DEG C toluene in, carry out decrement treatment using small model machine, processing time is 90min~120min, after decrement, after processing
CMA-PA/LDPE non-woven materials be submerged into DMF solvent, be cleaned by ultrasonic about 30min, place it in 50 DEG C again later
Ultrasonic washing is carried out in water, a not good liquor is changed at interval of 20min, and repetitive operation 3 times is finally taken out, and water is controlled, and low temperature drying both obtained
Collagen/PA materials.
5. a kind of preparation method of collagen according to claim 1/PA superfine fibre non-woven materials, feature exist
In in step 2, the use parameter of UV crosslinking instrument is：50W, 365nm, exposure chamber size 34cm × 26cm × l5cm, irradiation away from
From 15cm.
6. a kind of preparation method of collagen according to claim 1/PA superfine fibre non-woven materials, feature exist
In in step 1.2, the solid content of CMA solution is 6% ± 0.5%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304858A (en) * | 2011-07-28 | 2012-01-04 | 山东同大海岛新材料股份有限公司 | Preparation method of superfine fiber high-imitation grain synthetic leather |
| CN105862420A (en) * | 2016-06-06 | 2016-08-17 | 陕西科技大学 | Preparation method of modified sea-island ultra-fine fiber synthetic leather base cloth |
| CN106009011A (en) * | 2016-06-06 | 2016-10-12 | 陕西科技大学 | Method for preparing vinyl modified collagen membrane |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304858A (en) * | 2011-07-28 | 2012-01-04 | 山东同大海岛新材料股份有限公司 | Preparation method of superfine fiber high-imitation grain synthetic leather |
| CN105862420A (en) * | 2016-06-06 | 2016-08-17 | 陕西科技大学 | Preparation method of modified sea-island ultra-fine fiber synthetic leather base cloth |
| CN106009011A (en) * | 2016-06-06 | 2016-10-12 | 陕西科技大学 | Method for preparing vinyl modified collagen membrane |
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