CN109023577A - Build the preparation method of reinforced polypropylene nitrile chopped strand - Google Patents
Build the preparation method of reinforced polypropylene nitrile chopped strand Download PDFInfo
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- CN109023577A CN109023577A CN201710425432.0A CN201710425432A CN109023577A CN 109023577 A CN109023577 A CN 109023577A CN 201710425432 A CN201710425432 A CN 201710425432A CN 109023577 A CN109023577 A CN 109023577A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
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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
- 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
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
- C08F220/46—Acrylonitrile with carboxylic acids, sulfonic acids or salts thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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Abstract
The present invention relates to a kind of preparation methods for building reinforced polypropylene nitrile chopped strand, mainly solve the problems, such as polyacrylonitrile chopped strand enhancing cement material bending strength difference existing in the prior art.The present invention is by using the preparation method included the following steps: (1) prepared by precursor: spinning solution through measuring by coagulation forming, multistage solidification drawing-off, hot water drawing-off, washing, once oil, compacting by drying, steam drafting, thermal finalization, it is secondary oil, acquisition polyacrylonitrile fibre precursor after finish re-dry；(2) fiber is chopped: precursor carries out chopped by chopping machine, obtain building reinforced polypropylene nitrile chopped strand, wherein, acrylonitrile content≤5000ppm in spinning solution, polyacrylonitrile copolymer weight average molecular weight 100000-500000 in spinning solution, the technical solution of molecular weight distribution 2.0-5.0, preferably solves the problems, such as this, in the industrial production that can be used for building reinforced polypropylene nitrile chopped strand.
Description
Technical field
The present invention relates to a kind of preparation methods for building reinforced polypropylene nitrile chopped strand, more specifically, the present invention relates to
And a kind of preparation method of cement constructional material reinforced polypropylene nitrile chopped strand.
Background technique
Cement constructional material is a kind of widely used material, its good, price with the simple processability of construction technology
It is cheap, etc. a series of advantages building foundation, building wall and it is indoor in terms of be widely used.But simultaneously
There is also the disadvantages of easy to crack, brittleness is big, and it is a kind of widely used that organic or inorganic fiber is added in cement constructional material
Inhibit the method for cement material brittle cracking.
Can be used for the synthetic fibers that cement works reinforcing material uses has polyacrylonitrile fibre, aramid fiber, polypropylene fine
Dimension, vinal, carbon fiber, polyethylene fibre, polyester fiber, polyimide fiber etc..Polyacrylonitrile fibre has strong
The advantage that degree is suitable, cost performance is high is widely used in a variety of applications in cement constructional material.
Preparing polyacrylonitrile fibre as the one-step method of solvent using dimethyl sulfoxide has the advantages that spinning solution solid content is high
It is used in many enterprises.Cement constructional material reinforced polypropylene nitrile chopped strand preparation process include polymerization, de- list, deaeration,
Coagulation forming, multistage solidification drawing-off, multistage hot water drawing-off, washing, once oil, compacting by drying, steam drafting, thermal finalization,
It is secondary oil, finish re-dry, be chopped and etc..Each step in preparation process influence fibrous mechanical property, fiber with
The binding force of cement material eventually affects the service performance of cement enhancing construction material.
It polymerize stoste remaining acrylonitrile of institute after de- single, deaeration, significant shadow on the one hand is caused to in-situ production environment
It rings, another aspect institute residual propylene nitrile escapes during following process, forms hole in the fibre, and the inside for becoming fiber lacks
It falls into, is decreased obviously the mechanical property of fiber.The macromolecular structure for polymerizeing stoste is to prepare high-performance polyacrylonitrile chopped strand
Core, the most key parameter be weight average molecular weight and molecular weight distribution.It is worth noting that, acrylonitrile in spinning solution
Content control is too low, and will to will lead to de- single load big, increases production cost；And molecular weight is excessive and molecular weight distribution is narrow, it will
Cause spinning moulding difficult.
Japan Patent JP58120811A, JP60021905A, JP61163149A, JP06115989A, JP08003812A are public
The preparation process of 5 building reinforced polypropylene nitrile fibers is opened, but above-mentioned patent there is problems:
(1) be not known influence and final fiber of the acrylonitrile residual monomer in spinning solution to fiber process and its
Enhance the influence of cement material mechanical property；
(2) it is not known and prepares the most key macromolecular structure parameter-weight of high-strength building reinforced polypropylene nitrile fiber
Influence of the molecular weight and molecualr weight distribution to fiber and its enhancing cement material mechanical property.
In view of this, the present invention is specifically proposed.
Summary of the invention
Present invention mainly solves polyacrylonitrile chopped strand existing in the prior art enhancing cement material bending strength is poor
The problem of.The present invention preferably solves the problems, such as this by a kind of preparation method for building reinforced polypropylene nitrile chopped strand, has
Have the advantages that polyacrylonitrile chopped strand enhancing cement material bending strength is high.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows: a kind of building reinforced polypropylene nitrile is chopped
The preparation method of fiber, comprising the following steps:
(1) prepared by precursor: the spinning solution through measuring by coagulation forming, multistage solidification drawing-off, hot water drawing-off, washing,
It once oils, compacting by drying, steam drafting, thermal finalization, secondary oil, obtains polyacrylonitrile fibre precursor after finish is dry；
(2) fiber is chopped: precursor carries out chopped, acquisition building reinforced polypropylene nitrile chopped strand by chopping machine；
Wherein, acrylonitrile content is less than or equal to 5000ppm, polyacrylonitrile copolymer in spinning solution in the spinning solution
Weight average molecular weight 100000-500000, molecular weight distribution 2.0-5.0.
In above-mentioned technical proposal, the preferred 14-23%wt of spinning solution concentration；Polyacrylonitrile copolymer preferably includes third
The weight ratio of alkene nitrile and comonomer, acrylonitrile and comonomer is 98:2-99.8:0.02；Comonomer is preferably acrylic acid
One of esters, vinyl esters, acrylic amide, Sulfonates, ammonium salt class are a variety of, said combination can achieve one compared with
Good technical effect.
In above-mentioned technical proposal, acrylonitrile content is more preferably 20ppm≤acrylonitrile content in the spinning solution
≤ 5000ppm, more preferably 20ppm≤acrylonitrile content≤3000ppm, most preferably 50ppm≤acrylonitrile content≤
3000ppm。
In above-mentioned technical proposal, the coagulating bath medium is dimethyl sulphoxide aqueous solution, 10-70 DEG C of coagulation bath temperature, is coagulated
Admittedly bathing mass concentration 10-80%, draw ratio 0.5-0.9.
In above-mentioned technical proposal, the multiple tracks drawing-off that the multistage solidification drawing-off is 20-70 DEG C of temperature, draw ratio 1-2.
In above-mentioned technical proposal, the multiple tracks drawing-off that the hot water drawing-off is 90-99.5 DEG C of temperature, draw ratio 1-4.
In above-mentioned technical proposal, the washing is washed using 60-90 DEG C of multiple tracks of temperature, does not apply drawing-off in water-washing process.
In above-mentioned technical proposal, the compacting by drying temperature is 100-150 DEG C, draw ratio 0.9-1.0.
In above-mentioned technical proposal, the steam drafting absolute pressure is 0.1-1MPa, draw ratio 1-5.
In above-mentioned technical proposal, the heat setting temperature is 105-145 DEG C, draw ratio 0.92-1.0.
In above-mentioned technical proposal, 100-120 DEG C of temperature of the finish re-dry.
In above-mentioned technical proposal, a length of 3-32mm such as described chopped strand.
In above-mentioned technical proposal, further preferred scheme are as follows: 50ppm≤acrylonitrile content in the spinning solution≤
3000ppm, polyacrylonitrile copolymer weight average molecular weight 150000-350000, molecular weight distribution 2.0-4.5；The coagulating bath is situated between
Matter is dimethyl sulphoxide aqueous solution, 20-65 DEG C of coagulation bath temperature, coagulating bath mass concentration 15-75%, draw ratio 0.6-
0.85；The multiple tracks drawing-off that the multistage solidification drawing-off is 30-65 DEG C of temperature, draw ratio 1-1.5；The hot water drawing-off is temperature
90-99.5 DEG C of multiple tracks drawing-off, draw ratio 1-4；The washing is washed using 60-90 DEG C of multiple tracks of temperature, in water-washing process not
Apply drawing-off；The compacting by drying temperature is 100-145 DEG C, draw ratio 0.92-1.0；The steam drafting absolute pressure is
0.2-0.8MPa, draw ratio 2-5；The heat setting temperature is 105-140 DEG C, draw ratio 0.95-1.0；In the finish
105-120 DEG C of re-dry temperature；A length of 6-24mm such as the chopped strand.
By controlling acrylonitrile content in spinning solution in the present invention, acrylonitrile monemer is deposited in reduction fiber formation process
In the influence to Tensile strength of single fiber, the decline of Tensile strength of single fiber is avoided.Meanwhile passing through polyacrylonitrile in control spinning solution
Weight average molecular weight and molecular weight distribution further ensure that the filament strength of fiber, the polyacrylonitrile of acquisition in suitable range
It is high that chopped strand enhances cement material bending strength.
It is spun using technical solution of the present invention due to using 20ppm≤acrylonitrile content≤5000ppm in spinning solution
Polyacrylonitrile copolymer weight average molecular weight 100000-500000 in silk stock solution, the spinning solution of molecular weight distribution 2.0-5.0, this
The matching of three elements has preferable synergistic function, so that thus obtained chopped strand enhancing cement material bending is strong
It spends up to 11MPa, achieves preferable technical effect.
The present invention is further elaborated below by embodiment.
Specific embodiment
[embodiment 1]
1, spinning solution: acrylonitrile, methylpropenyl sodium sulfonate, methyl acrylate example 99.6 in mass ratio will be refined:
0.1:0.3, solid content 15%, azodiisobutyronitrile account for comonomer 0.1wt%, are added to reaction by solvent of dimethyl sulfoxide
In device, weight average molecular weight 450000 is obtained, the polymerization stoste of molecular weight distribution 4.6 obtains after taking off single, deaeration containing 5000ppm third
The residual single stoste of alkene nitrile, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: using wet spinning carry out as-spun fibre preparation, spinning solution through metering pump accurate measurement, again
After filtering, entered in the first coagulating bath by spinneret, 25 DEG C of setting temperature, concentration 75wt%, draw ratio 0.85 is subsequent
It carries out two-stage and solidifies drawing-off, draw ratio is respectively 1.05,1.1, obtains coagulated fibre.
3, drawing-off and washing: three hot water drawing temperatures are respectively 90,98,99 DEG C, draw ratio is respectively 1.8,2.0,
2.4；65 DEG C of the road 1-3 washing temperature, 75 DEG C of the road 4-6 washing temperature, 80 DEG C of the road 7-9 washing temperature.
4, once oil and compacting by drying: the fiber that step 3 is obtained carries out compacting by drying after once being oiled,
Compacting by drying temperature is in ladder-elevating temperature mode, and the 1st 100 DEG C of compacting by drying temperature, the 2nd compacting by drying temperature is
140℃。
5, steam drafting and thermal finalization: the fiber that step 4 is obtained carries out 3.5 times of drawing-offs in the steam of 0.7MPa, it
Thermal finalization, thermal finalization draw ratio 0.98 are carried out in 130 DEG C of steam afterwards.
6, secondary to oil and finish re-dry: the fiber that step 5 obtains is oiled and finish re-dry by secondary.
7, fiber is chopped: the fiber that step 6 obtains being chopped and is prepared into 12mm long chopped strand, test fibre single thread is strong
Degree.
8, chopped strand prepared by step 7 2% the preparation of fiber reinforced cement material: is added to cement bonded sand by volume
In slurry, it is prepared into 230mm × 100mm × 9mm sample, is solidified in 25 DEG C, relative humidity 95% or so, after solidification
The bending strength of test sample.
The bending strength that test obtains fiber reinforced cement mortar material is 10.5MPa.
[embodiment 2]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 100000 be made, molecular weight distribution 5
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10MPa.
[embodiment 3]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 500000 be made, molecular weight distribution 5
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.5MPa.
[embodiment 4]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 100000 be made, molecular weight distribution 2
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.1MPa.
[embodiment 5]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 150000 be made, molecular weight distribution 2
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 3000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.3MPa.
[embodiment 6]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 150000, molecular weight distribution 4.5 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 3000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.2MPa.
[embodiment 7]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 350000 be made, molecular weight distribution 2
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 3000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 11MPa.
[embodiment 8]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 350000, molecular weight distribution 4.5 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 3000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.7MPa.
[embodiment 9]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 300000 be made, molecular weight distribution 3
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 200ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.8MPa.
[embodiment 10]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 150000 be made, molecular weight distribution 2
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 2000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.6MPa.
[embodiment 11]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 350000, molecular weight distribution 4.5 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 2000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.8MPa.
[embodiment 12]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 300000, molecular weight distribution 2.7 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 3500ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 10.5MPa.
[comparative example 1]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 70000, molecular weight distribution 2.5 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 8.0MPa.
[comparative example 2]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 100000, molecular weight distribution 4.5 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 7000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 8.5MPa.
[comparative example 3]
1, spinning solution: being formulated using the identical copolymerization of embodiment 1, weight average molecular weight 150000 be made, molecular weight distribution 6
It polymerize stoste, obtains the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, 2 microns of secondary filters obtain spinning solution.
2, coagulation forming: with 1 step 2 of embodiment.
3, drawing-off and washing: with 1 step 3 of embodiment.
4, it once oils and compacting by drying: with 1 step 4 of embodiment.
5, steam drafting and thermal finalization: with 1 step 5 of embodiment.
6, secondary to oil and finish re-dry: with 1 step 6 of embodiment.
7, fiber is chopped: with 1 step 7 of embodiment.
8, the preparation of fiber reinforced cement mortar material: with 1 step 8 of embodiment.
The bending strength that test obtains fiber reinforced cement mortar material is 8.9MPa.
[comparative example 4]
1, it spinning solution: is formulated using the identical copolymerization of embodiment 1, weight average molecular weight 450000, molecular weight distribution 4.6 is made
Polymerization stoste, obtain the residual single stoste of acrylonitrile containing 5000ppm after taking off single, deaeration, it is former that 2 microns of secondary filters obtain spinning
Liquid.
2, coagulation forming: using wet spinning carry out as-spun fibre preparation, spinning solution through metering pump accurate measurement, again
After filtering, entered in the first coagulating bath by spinneret, 25 DEG C of setting temperature, concentration 75wt%, draw ratio 0.85 is subsequent
It carries out two-stage and solidifies drawing-off, draw ratio is respectively 1.05,1.1, obtains coagulated fibre.
3, drawing-off and washing: three hot water drawing temperatures are respectively 90,98,99 DEG C, draw ratio is respectively 1.8,2.0,
2.4；65 DEG C of the road 1-3 washing temperature, 75 DEG C of the road 4-6 washing temperature, 80 DEG C of the road 7-9 washing temperature.
4, two oil and compacting by drying: the fiber that step 3 is obtained carries out first and dry causes after once being oiled
Densification, 100 DEG C of compacting by drying temperature, then carry out it is secondary oil, the 2nd compacting by drying temperature be 140 DEG C.
5, steam drafting and thermal finalization: the fiber that step 4 is obtained carries out 3.5 times of drawing-offs in the steam of 0.7MPa, it
Thermal finalization, thermal finalization draw ratio 0.98 are carried out in 130 DEG C of steam afterwards.
6, fiber is chopped: the fiber that step 5 obtains being chopped and is prepared into 12mm long chopped strand.
Test obtains fiber and mixes in cement material unevenly.
[comparative example 5]
1, spinning solution: purification acrylonitrile, itaconic acid are pressed into 97:3 (wt%), weight average molecular weight 150000, molecule is made
The polymerization stoste of amount distribution 4.3 obtains the residual single stoste of acrylonitrile containing 3000ppm after taking off single, deaeration, and 2 microns of secondary filters obtain
Obtain spinning solution.
2, coagulation forming: using wet spinning carry out as-spun fibre preparation, spinning solution through metering pump accurate measurement, again
After filtering, entered in the first coagulating bath by spinneret, 25 DEG C of setting temperature, concentration 75wt%, draw ratio 0.85 is subsequent
It carries out two-stage and solidifies drawing-off, draw ratio is respectively 1.05,1.1, obtains coagulated fibre.
3, drawing-off and washing: three hot water drawing temperatures are respectively 90,98,99 DEG C, draw ratio is respectively 1.8,2.0,
2.4；65 DEG C of the road 1-3 washing temperature, 75 DEG C of the road 4-6 washing temperature, 80 DEG C of the road 7-9 washing temperature.
4, two oil and compacting by drying: the fiber that step 3 is obtained carries out first and dry causes after once being oiled
Densification, 100 DEG C of compacting by drying temperature, then carry out it is secondary oil, the 2nd compacting by drying temperature be 140 DEG C.
5, steam drafting and thermal finalization: the fiber that step 4 is obtained carries out 3.5 times of drawing-offs in the steam of 0.7MPa, it
Thermal finalization, thermal finalization draw ratio 0.98 are carried out in 130 DEG C of steam afterwards.
6, fiber is chopped: the fiber that step 5 obtains being chopped and is prepared into 12mm long chopped strand.
The bending strength that test obtains fiber reinforced cement mortar material is 9.0MPa.
Claims (10)
1. a kind of preparation method for building reinforced polypropylene nitrile chopped strand, comprising the following steps:
(1) prepared by precursor: the spinning solution through measuring by coagulation forming, multistage solidification drawing-off, multistage hot water drawing-off, washing,
Once oil, compacting by drying, steam drafting, thermal finalization, it is secondary oil, that polyacrylonitrile fibre is obtained after finish re-dry is former
Silk；
(2) fiber is chopped: precursor carries out chopped, acquisition building reinforced polypropylene nitrile chopped strand by chopping machine；
Wherein, acrylonitrile content is less than or equal to 5000ppm, polyacrylonitrile copolymer Weight-average molecular in spinning solution in spinning solution
Measure 100000-500000, molecular weight distribution 2.0-5.0.
2. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that described solidifying
Admittedly bath medium is dimethyl sulphoxide aqueous solution, 10-70 DEG C of coagulation bath temperature, coagulating bath mass concentration 10-80%, draw ratio is
0.5-0.9。
3. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that described more
The multiple tracks drawing-off that grade solidification drawing-off is 20-70 DEG C of temperature, draw ratio 1-2.
4. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that the heat
The multiple tracks drawing-off that water drawing-off is 90-99.5 DEG C of temperature, draw ratio 1-4.
5. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that the water
It washes and is washed using 60-90 DEG C of multiple tracks of temperature, do not apply drawing-off in water-washing process.
6. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that described dry
Dry densification temperature is 100-150 DEG C, draw ratio 0.9-1.0.
7. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that the steaming
Vapour drawing-off absolute pressure is 0.1-1MPa, draw ratio 1-5.
8. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that the heat
Setting temperature is 105-145 DEG C, draw ratio 0.92-1.0.
9. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that the oil
100-120 DEG C of temperature of agent re-dry.
10. the preparation method of building reinforced polypropylene nitrile chopped strand according to claim 1, it is characterised in that described short
Cut a length of 3-32mm such as fiber.
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Cited By (3)
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| CN110863256A (en) * | 2019-10-29 | 2020-03-06 | 江苏恒神股份有限公司 | Preparation method of dry-jet wet-spun high-strength medium-modulus polyacrylonitrile-based carbon fiber precursor |
| CN111118680A (en) * | 2019-08-26 | 2020-05-08 | 张昌录 | High-elasticity wear-resistant fiber fabric |
| CN114481349A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Preparation method of high-strength alkali-resistant polyacrylonitrile fiber and polyacrylonitrile fiber |
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| CN111118680A (en) * | 2019-08-26 | 2020-05-08 | 张昌录 | High-elasticity wear-resistant fiber fabric |
| CN110863256A (en) * | 2019-10-29 | 2020-03-06 | 江苏恒神股份有限公司 | Preparation method of dry-jet wet-spun high-strength medium-modulus polyacrylonitrile-based carbon fiber precursor |
| CN110863256B (en) * | 2019-10-29 | 2022-05-31 | 江苏恒神股份有限公司 | Preparation method of dry-jet wet-spun high-strength medium-modulus polyacrylonitrile-based carbon fiber precursor |
| CN114481349A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Preparation method of high-strength alkali-resistant polyacrylonitrile fiber and polyacrylonitrile fiber |
| CN114481349B (en) * | 2020-10-26 | 2024-01-30 | 中国石油化工股份有限公司 | Preparation method of high-strength alkali-resistant polyacrylonitrile fiber and polyacrylonitrile fiber |
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Application publication date: 20181218 |