CN103160952A - Preparation method of fiber with high water absorption - Google Patents
Preparation method of fiber with high water absorption Download PDFInfo
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- CN103160952A CN103160952A CN2013101298329A CN201310129832A CN103160952A CN 103160952 A CN103160952 A CN 103160952A CN 2013101298329 A CN2013101298329 A CN 2013101298329A CN 201310129832 A CN201310129832 A CN 201310129832A CN 103160952 A CN103160952 A CN 103160952A
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Abstract
The invention relates to a preparation method of a fiber with high water absorption, which is a method for preparing the fiber with high water absorption by a post-crosslinking agent. According to the preparation method, the fiber with high water absorption is prepared from acrylic acid (AA) and acrylamide (AM) which are partly neutralized and taken as polymerized monomers through the steps of: blending the polymerized monomers with polyving akohol (PVA), initiating by potassium persulfate (KPS), blending and polymerizing in an aqueous solution, adding a dialdehyde solution to obtain a mixed solution serving as a post-crosslinking agent solution, mixing to be uniform and defoaming to obtain a spinning stock solution; dry-wet spinning the spinning stock solution to form a nascent fiber; and heat-treating the nascent fiber at a certain temperature to generate a crosslinking reaction, thereby forming the three-dimensional net-structured fiber with high water absorption. According to the preparation method, the implosion phenomenon which easily occurs during polymerization of the traditional polymer solution with high water absorption is avoided, the preparation technology is simple and safe, the production cost is reduced, and the production efficiency is increased; and the obtained water-absorbing fiber has high and controllable water adsorption, thermostability, capability of being repeatedly used, and long residual action.
Description
Technical field
The present invention relates to a kind of preparation method of high water-absorption fiber, particularly relate to a kind of preparation method of rear crosslinked high water-absorption fiber, specifically a kind of dry-wet spinning preparation method of rear cross-linking type high water-absorption fiber.
Background technology
High water-absorption fiber is after high hydroscopic resin, the specific function fiber that grows up, and it is extension and the expansion of high hydroscopic resin.Because high water-absorption fiber has many superiority, high very active to the research of water-absorption fiber both at home and abroad.The producing country of high water-absorption fiber mainly contains Canada, Japan, the U.S., Britain, Germany etc. at present, and domestic starting is more late, but also presents in recent years development trend fast.
Britain Technical Absorbents company development and be to carry out aqueous solution polymerization take acrylic acid and vinyl unsaturated monomer as raw material with " Bell Oasis " fiber that Japanese clock spins company's co-production, through [the work of field, natural pond length that dry spinning is shaped, heat cross-linking is made, Chen Longyun translates, high suction water absorbent fiber BELL OASIS, the Overseas Textile Industry technology, 2002,4:7～9]." Fibersorb " fiber that US Patent No. P5026784 document is announced is the high water-absorption fiber of U.S. Acro chemical technology company research and development.
China Textile Academy's publication number be the patent of CN1407147 be with acrylic acid, sodium acrylate and acrylate etc. together in the aqueous solution polymerization obtain aqueous copolymers solution, take polyvinyl alcohol water solution as sandwich layer or cortex, through the sheath-core type composite spinneret extrude, hot-air dry spinning and heat cross-linking obtain high water-absorption fiber.Sheath-core type composite fibre preparing technique process is complicated, and equipment cost increases.
Document " microstructure and the imbibition ability of PVA/PAA-AM blend high water-absorption fiber " (fine chemistry industry, 2005,22 (3): 177～180) with acrylic acid, acrylamide monomer copolymerization, with polyvinyl alcohol blending, carry out solution wet spinning by the self-control spinning machine under N2 pressure, acetone is coagulating bath, the preparation high water-absorption fiber, the high energy of its water absorption rate reaches 243g/g, inhales the salt solution multiplying power and is up to 58g/g.
Document " acrylic acid-acrylamide copolymer fibre and water absorbing properties research thereof " (thesis for the doctorate, 2006) with acrylic acid, acrylamide monomer copolymerization, prepare high water-absorption fiber with polyvinyl alcohol blending, this article record: adopt and introduce the latent crosslinker N hydroxymethyl acrylamide in acrylic acid, acrylamide, polyvinyl alcohol polymerization system, polymerisation in solution obtains high water-absorption fiber by wet spinning, heat cross-linking.Wherein crosslinking agent is just to add when raw material propylene acid, acrylamide monomer copolymerization, when polymerization, the part cross-linking reaction can occur, and easily causes sudden and violent poly-.
Although above prior art prepares high water-absorption fiber with the acrylic acid of part neutralization and the aqueous solution spinning of acrylamide and polyvinyl alcohol blending, but the autoacceleration effect when in fact the interpolation of crosslinking agent can aggravate polymerization before polymerization, when monomer polymerization enters the autoacceleration state, the instantaneous increase of viscosity in polymerization system, the heat of polymerization that produces easily gathers and causes at last cruelly gathering phenomenon.Although it is rear crosslinked to use some latent crosslinkers to carry out, but also just a part is rear crosslinked, crosslinking agent still can react in polymerization, be difficult to control the degree of cross linking, make copolymerizing and blending solution unstable, the final stability that affects high water-absorption fiber, resulting high water-absorption fiber water absorbing properties is not high enough, can not meet the requirement that some need the high mixed fine fabric of water absorption rate, medical dressing etc.In addition, as-spun fibre does not form cross-linked structure, poor mechanical property, and wet spinning is easily disconnected fine in the preparation high water-absorption fiber, affects production efficiency.
Summary of the invention
The objective of the invention is for prior art not enoughly and a kind of preparation method of high water-absorption fiber is provided, described fiber has three-dimensional net structure, and water absorbent rate is controlled, and physical and mechanical properties is good, and described preparation method's process stabilizing, cost are low.
To achieve these goals, technical scheme provided by the invention is, a kind of preparation method of high water-absorption fiber, adopted acrylic acid and acrylamide as polymerization single polymerization monomer, polyvinyl alcohol is polymer blend, sneak into dialdehyde crosslinking agent solution after polymerisation in solution is completed and prepare spinning solution, through the dry-wet spinning fibroblast, then heat cross-linking obtains high water-absorption fiber of the present invention.
The technical scheme that the present invention solves described high water-absorption fiber technical problem is:
The preparation method of a kind of high water-absorption fiber of the present invention comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Polyvinyl alcohol 2～8 weight portions are dissolved in the deionized water of 50～80 weight portions, are heated to 95～100 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 15～30 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 60～80%, then adds acrylamide 5～10 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
The acrylate moiety neutralization is in order to reduce the speed of acrylic acid and acrylamide copolyreaction, to avoid the sudden and violent poly-phenomenon of the too fast generation of reaction.
C. the preparation of initiator solution C
0.1～2 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 10～20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The dialdehyde of 0.5～5 weight portion is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 40～50 ℃ of conditions, be warmed up to again 50～65 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 65～80 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 3～8 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
Add described initiator solution C at 50～65 ℃, efficiency of initiator is high, and during polymerization, low polymerization time is long for temperature, and polymerization temperature height polymerization time is short, cruelly gathers phenomenon when adding cross-linking agent solution D to avoid polymerization when reaction finishes.
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter from the spinning head ejection, enters acetone coagulating bath solidification forming after the air layer of dynamic analysis of spinning through 10～50mm, make as-spun fibre in 70～90 ℃;
70～90 ℃ of mobility that can improve solution through measuring pump, be easy to spinning technique.Dynamic analysis of spinning can improve stretch orientation and the condensation rate of fiber through air layer, improves spinning efficiency.
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch typing and heat cross-linking successively process, obtain high water-absorption fiber;
Described hot-stretch is processed: 100～150 ℃ of draft temperatures, stretch 1.5～2.5 times, and 2～10 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 120～180 ℃, heat cross-linking time 30s～30mins.
As preferred technical scheme:
The preparation method of a kind of high water-absorption fiber as above, described dialdehyde be glyoxal, any in malonaldehyde, butanedial or glutaraldehyde.
The preparation method of a kind of high water-absorption fiber as above, the mass concentration of described spinning solution are 16～28%.
The preparation method of a kind of high water-absorption fiber as above, the temperature of described acetone coagulating bath are 5～25 ℃; Setting time is 3～8mins.
The preparation method of a kind of high water-absorption fiber as above, the orifice diameter of described spinning head are Φ 0.1～1mm, and the spinneret orifice quantity of single spinning head is 1～1000 hole.
The preparation method of a kind of high water-absorption fiber as above, the degree of polymerization of described polyvinyl alcohol are 1000～3000, and alcoholysis degree is 80～99%.
The preparation method of a kind of high water-absorption fiber as above, it is 100～500g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 20～150g/g.
Beneficial effect:
1, rear crosslinking agent method improves polymerisation and product stability
usually adopt one-step polymerization method in prior art, all raw materials are comprised that latent crosslinker sneaks into together copolymerizing and blending and obtain spinning solution, but phenomenon very easily occurs cruelly to gather in two stages of the chain growth of polymerization, partial reaction produces cross-linked structure and heat of polymerization seriously gathered because can occur when polymerization latent crosslinker, sudden and violent poly-phenomenon occurs in autoacceleration effect aggravation, even strict control temperature and fed batch are to slow down the autoacceleration effect in polymerization process, but each of gained batch copolymerized blend unstable properties, be difficult to prepare the degree of cross linking and be evenly water absorbing properties controlled the high water-absorption fiber product, and the copolymerizing and blending solution spinnability with cross-linked structure is bad.
and the present invention has adopted acrylic acid and acrylamide as polymerization single polymerization monomer, polyvinyl alcohol is polymer blend, sneak into crosslinking agent dialdehyde solution after polymerisation in solution is completed and prepare spinning solution, dialdehyde be after fibroblast with polyvinyl alcohol generation crosslinked action, when this synthetic technology route can alleviate polymerization greatly, thereby the autoacceleration effect avoids cruelly gathering the generation of phenomenon, the copolymerized blend of gained is linear structure, the solution spinnability is better, dialdehyde and polyvinyl alcohol generation cross-linking reaction after fibroblast, in conjunction with bond energy larger, after the fiber suction, gel strength is high, can keep fibre morphology, the fiber hot water resistance can, thereby and can control the degree of cross linking according to dialdehyde content and control water absorption rate.
2, the dry-wet spinning method is enhanced productivity and properties of product
Usually adopt dry spinning or wet spinning technology in prior art, the dry spinning fibroblast is effective, but cost is high, and spun fiber more smoothly do not have microcellular structure, is unfavorable for improving the water imbibition of high water-absorption fiber.Wet spinning is easily disconnected fine, and also do not carry out the exploration of dry-wet spinning at present for height suction copolymerized blend solution, the present invention adopts the dry-wet spinning technology, after spinning solution flows out spinneret orifice, first by air layer, so just can greatly improve spinneret draft, thereby the high 5-10 of the comparable general wet spinning of spinning speed doubly, the spinnerets hole count is more than dry spinning spinnerets hole count in addition, has greatly improved production efficiency.
In addition, in the dry-wet spinning process, dynamic analysis of spinning has the effect of stretch orientation in by air event, has greatly strengthened the mechanical property of as-spun fibre, does not allow easily broken fibre in spinning process.
The technology of the present invention can alleviate polymerization autoacceleration effect to a great extent, makes spinning solution stable, and the high water-absorption fiber physical and mechanical properties that makes is good, water absorption rate improve and controlled, suction after high, the hot water resistance of gel strength.Rear cross-linking type high water-absorption fiber of the present invention adopts the dry-wet spinning technology of preparing, and the preparation method is simple, steady quality, efficient is high, cost is lower, is convenient to industrializing implementation.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 3000 with the degree of polymerization, polyvinyl alcohol 2 weight portions of alcoholysis degree 99% are dissolved in the deionized water of 50 weight portions, are heated to 100 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 15 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 60%, then adds acrylamide 5 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
0.1 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 10 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glyoxal of 0.5 weight portion is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 40 ℃ of conditions, be warmed up to again 50 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 65 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 8 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 70 ℃, and the orifice diameter of described spinning head is Φ 0.1mm, and the spinneret orifice quantity of single spinning head is 1000 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 10mm, and the temperature of described acetone coagulating bath is 5 ℃, and setting time is 3mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 487g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 136g/g;
Described hot-stretch is processed: 100 ℃ of draft temperatures, stretch 1.5 times, and 2 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 120 ℃, heat cross-linking time 30mins.
Embodiment 2
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1700 with the degree of polymerization, polyvinyl alcohol 8 weight portions of alcoholysis degree 88% are dissolved in the deionized water of 80 weight portions, are heated to 95 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 30 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 80%, then adds acrylamide 10 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
2 weight portion potassium peroxydisulfates are dissolved in obtain initiator solution C in 20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glutaraldehyde of 5 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 50 ℃ of conditions, be warmed up to again 65 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 80 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 3 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 90 ℃, and the orifice diameter of described spinning head is Φ 1mm, and the spinneret orifice quantity of single spinning head is 1 hole; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 50mm, and the temperature of described acetone coagulating bath is 25 ℃, and setting time is 8mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 500g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 150g/g;
Described hot-stretch is processed: 150 ℃ of draft temperatures, stretch 2.5 times, and 10 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 180 ℃, heat cross-linking time 30s.
Embodiment 3
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1800 with the degree of polymerization, polyvinyl alcohol 6 weight portions of alcoholysis degree 99% are dissolved in the deionized water of 70 weight portions, are heated to 98 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 18 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 70%, then adds acrylamide 8 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
1 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 15 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The malonaldehyde of 3 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 45 ℃ of conditions, be warmed up to again 55 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 70 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 5 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 80 ℃, and the orifice diameter of described spinning head is Φ 0.5mm, and the spinneret orifice quantity of single spinning head is 10 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 30mm, and the temperature of described acetone coagulating bath is 15 ℃, and setting time is 5mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 464g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 122g/g;
Described hot-stretch is processed: 120 ℃ of draft temperatures, stretch 2.5 times, and 6 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 150 ℃, heat cross-linking time 14mins.
Embodiment 4
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1700 with the degree of polymerization, polyvinyl alcohol 7 weight portions of alcoholysis degree 92% are dissolved in the deionized water of 70 weight portions, are heated to 95 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 25 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 70%, then adds acrylamide 7 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
1.5 weight portion potassium peroxydisulfates are dissolved in obtain initiator solution C in 15 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The butanedial of 2 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 48 ℃ of conditions, be warmed up to again 60 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 75 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 4 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 80 ℃, and the orifice diameter of described spinning head is Φ 0.2mm, and the spinneret orifice quantity of single spinning head is 100 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 20mm, and the temperature of described acetone coagulating bath is 15 ℃, and setting time is 5mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 250g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 62g/g;
Described hot-stretch is processed: 130 ℃ of temperature, stretch 2 times, and 5 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 160 ℃, heat cross-linking time 3mins.
Embodiment 5
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1700 with the degree of polymerization, polyvinyl alcohol 6 weight portions of alcoholysis degree 99% are dissolved in the deionized water of 75 weight portions, are heated to 96 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 18 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 65%, then adds acrylamide 9 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
0.6 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 18 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glutaraldehyde of 4 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 50 ℃ of conditions, be warmed up to again 55 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 68 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 4.5 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 80 ℃, and the orifice diameter of described spinning head is Φ 0.15mm, and the spinneret orifice quantity of single spinning head is 400 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 20mm, and the temperature of described acetone coagulating bath is 10 ℃, and setting time is 4mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 371g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 92g/g;
Described hot-stretch is processed: 140 ℃ of draft temperatures, stretch 2 times, and 5 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 170 ℃, heat cross-linking time 1mins.
Embodiment 6
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1000 with the degree of polymerization, polyvinyl alcohol 6 weight portions of alcoholysis degree 95% are dissolved in the deionized water of 75 weight portions, are heated to 98 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 26 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 75%, then adds acrylamide 8 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
0.15 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glutaraldehyde of 3 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 48 ℃ of conditions, be warmed up to again 60 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 75 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 4.5 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 80 ℃, and the orifice diameter of described spinning head is Φ 0.5mm, and the spinneret orifice quantity of single spinning head is 36 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 40mm, and the temperature of described acetone coagulating bath is 10 ℃, and setting time is 5mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 301g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 67g/g;
Described hot-stretch is processed: 110 ℃ of temperature, stretch 2 times, and 5 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 130 ℃, heat cross-linking time 17mins.
Embodiment 7
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1700 with the degree of polymerization, polyvinyl alcohol 8 weight portions of alcoholysis degree 99% are dissolved in the deionized water of 75 weight portions, are heated to 98 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 30 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 75%, then adds acrylamide 13 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
0.15 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glutaraldehyde of 1.5 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 45 ℃ of conditions, be warmed up to again 55 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 75 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 4.5 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 80 ℃, and the orifice diameter of described spinning head is Φ 0.8mm, and the spinneret orifice quantity of single spinning head is 10 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 30mm, and the temperature of described acetone coagulating bath is 10 ℃, and setting time is 5mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 188g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 57g/g;
Described hot-stretch is processed: 120 ℃ of temperature, stretch 1.5 times, and 8 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 150 ℃, heat cross-linking time 15mins.
Embodiment 8
A kind of preparation method of high water-absorption fiber comprises the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A
Be 1000 with the degree of polymerization, polyvinyl alcohol 8 weight portions of alcoholysis degree 80% are dissolved in the deionized water of 75 weight portions, are heated to 98 ℃ and stir the formation solution A;
B. the preparation of monomer solution B
The acrylic acid of 30 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 75%, then adds acrylamide 15 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C
1.2 weight portion potassium peroxydisulfates are dissolved in obtain initiator solution C in 20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D
The glyoxal of 1.5 weight portions is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution
Described monomer solution B is dispersed in described solution A, mix under 45 ℃ of conditions, be warmed up to again 55 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 80 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 3.5 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter sprays from spinning head in 85 ℃, and the orifice diameter of described spinning head is Φ 0.3mm, and the spinneret orifice quantity of single spinning head is 800 holes; Dynamic analysis of spinning enters acetone coagulating bath solidification forming through after the air layer of 30mm, and the temperature of described acetone coagulating bath is 10 ℃, and setting time is 5mins, makes as-spun fibre;
(4) post processing of as-spun fibre
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber, it is 100g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 20g/g;
Described hot-stretch is processed: 120 ℃ of temperature, stretch 1.5 times, and 8 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 130 ℃, heat cross-linking time 25mins.
Claims (7)
1. the preparation method of a high water-absorption fiber is characterized in that comprising the following steps:
(1) solution is prepared, each material by weight:
A. the preparation of solution A;
Polyvinyl alcohol 2～8 weight portions are dissolved in the deionized water of 50～80 weight portions, are heated to 95～100 ℃ and stir the formation solution A;
B. the preparation of monomer solution B;
The acrylic acid of 15～30 weight portions is neutralized with sodium hydroxide solution, and degree of neutralization is 60～80%, then adds acrylamide 5～10 weight portions, mixes under room temperature and obtains monomer solution B; Described degree of neutralization refers to that sodium acrylate weight multiply by 100% again divided by sodium acrylate and acrylic acid weight sum;
C. the preparation of initiator solution C;
0.1～2 weight portion potassium peroxydisulfate is dissolved in obtains initiator solution C in 10～20 parts by weight of deionized water;
D. the preparation of cross-linking agent solution D;
The dialdehyde of 0.5～5 weight portion is dissolved in 20 parts by weight of deionized water under room temperature, obtains cross-linking agent solution D;
(2) preparation of spinning solution;
Described monomer solution B is dispersed in described solution A, mix under 40～50 ℃ of conditions, be warmed up to again 50～65 ℃ and add described initiator solution C, logical nitrogen, be warmed up to 65～80 ℃ of reactions and obtained polyacrylic acid-acrylamide/polyvinyl alcohol copolymerizing and blending solution in 3～8 hours, add described cross-linking agent solution D to mix after reaction finishes and obtain spinning solution;
(3) dry-wet spinning of spinning solution;
Spinning solution is carried out pressure filtration, deaeration, through measuring pump, filter from the spinning head ejection, enters acetone coagulating bath solidification forming after the air layer of dynamic analysis of spinning through 10～50mm, make as-spun fibre in 70～90 ℃;
(4) post processing of as-spun fibre;
As-spun fibre is carried out hot-stretch and heat cross-linking successively process, obtain high water-absorption fiber;
Described hot-stretch is processed: 100～150 ℃ of draft temperatures, stretch 1.5～2.5 times, and 2～10 minutes time;
Described heat cross-linking is processed: the heat cross-linking temperature is 120～180 ℃, heat cross-linking time 30s～30mins.
2. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, described dialdehyde be glyoxal, any in malonaldehyde, butanedial or glutaraldehyde.
3. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, the mass concentration of described spinning solution is 16～28%.
4. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, the temperature of described acetone coagulating bath is 5～25 ℃; Setting time is 3～8mins.
5. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, the orifice diameter of described spinning head is Φ 0.1～1mm, and the spinneret orifice quantity of single spinning head is 1～1000 hole.
6. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, the degree of polymerization of described polyvinyl alcohol is 1000～3000, and alcoholysis degree is 80～99%.
7. the preparation method of a kind of high water-absorption fiber according to claim 1, is characterized in that, it is 100～500g/g that described high water-absorption fiber sucks the ionized water multiplying power, inhales physiological saline 20～150g/g.
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