CN103060940B - A kind of preparation method of medium modulus vinal - Google Patents
A kind of preparation method of medium modulus vinal Download PDFInfo
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- CN103060940B CN103060940B CN201110316862.1A CN201110316862A CN103060940B CN 103060940 B CN103060940 B CN 103060940B CN 201110316862 A CN201110316862 A CN 201110316862A CN 103060940 B CN103060940 B CN 103060940B
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Abstract
A kind of preparation method of medium modulus PVA fiber, first by raw material mixed dissolution, carry out conventional wet lay spinning again and obtain PVA fiber, it is characterized in that: described raw material comprises PVA, imvite and water, wherein PVA accounts for 100 parts, imvite accounts for 1 ~ 20 part, water accounts for 400 ~ 800 parts.PVA fiber producing processes of the present invention is compared with high strength high modulus PVA fiber technique, simple to operate, with low cost, has more the feature of environmental protection, is particularly suitable for industrialization large-scale production.The PVA fiber linear density that the present invention obtains is 1.0 ~ 10.0dtex, dry fracture strength 6.0 ~ 10.0cN/dtex, extension at break 6 ~ 20%, Young's modulus 110 ~ 200cN/dtex; Be highly suitable in building field or industrial cloth and apply.
Description
Technical field
The present invention relates to the preparation method of vinal, particularly relate to a kind of method preparing medium modulus vinal.
Background technology
Vinal (hereinafter referred to as PVA fiber) is as a kind of corrosion resistance, weather fastness and the macromolecular material with base material bonds well performance, and its purposes is quite extensive, except making asbestos substitute, tire cord, industry cloth etc.Because its good pardon, also can be mixed into various functional filler spinning in PVA stoste, meet the different market demands.
The method preparing PVA fiber is mainly wet spinning, and it comprises conventional wet lay spinning technique and high-strength high-modulus fibre spinning technique.Conventional wet lay spinning is after PVA stoste sprays from spinning head, coagulation forming in saturated metabisulfite solution, then obtains fiber by post processing, and the fiber Young's modulus that this method obtains is approximately 40 ~ 110cN/dtex.High-strength high-modulus fibre spinning technique be with the addition of boric acid PVA stoste thread by alkaline bath (NaOH and metabisulfite solution) cross moulding, remove crosslinked again through acid bath (sulfuric acid and sodium sulphate mixed solution), then process is washed for a long time, obtain high-modulus PVA fiber finally by high power hot-stretch, the method obtains fiber modulus at more than 180cN/dtex; But its disadvantage is: relate to strong acid and strong base in spinning process, and operational danger is large; Washing time is very long, and energy consumption is high, does not possess advantage when therefore preparing the fiber of some medium modulus in this way.
More a kind of functional filler is reported in imvite in recent years, it has unique stratiform one-dimensional nano structure characteristic and morphological character, interlayer has programmable reactivity, the specific area of super large and up to more than 200 footpath/thickness rate, this structure will give the physical and mechanical properties of polymer-montmorillonoid composite excellence.But the application of imvite in the preparation of PVA fiber has not yet to see report.
Summary of the invention
The object of the present invention is to provide the medium modulus PVA fiber producing processes that a kind of security is good, easy and simple to handle.
Object of the present invention is realized by following technical measures, and wherein said raw material number, except specified otherwise, is parts by weight.
A kind of preparation method of medium modulus PVA fiber, first by raw material mixed dissolution, carry out conventional wet lay spinning again and obtain PVA fiber, it is characterized in that: described raw material comprises PVA, imvite and water, wherein PVA accounts for 100 parts, imvite accounts for 1 ~ 20 part, water accounts for 400 ~ 800 parts.
The present invention adopts the imvite of above-mentioned amount to be distributed in PVA stoste as the raw material preparing PVA fiber dexterously, discovery can adopt conventional wet lay spinning technique just can obtain the PVA fiber (the PVA fiber Young's modulus of acquisition is 110 ~ 190cN/dtex) of medium modulus, its technique is simple, security good, with low cost, be particularly suitable for industrial-scale production.
In order to improve the uniformity of final PVA fiber, obtain that quality is more stable, the better PVA fiber of commodity property, further preferably, above-mentioned each raw material is PVA 100 parts, imvite accounts for 17 parts, water accounts for 650 ~ 680 parts.
More preferably, in above-mentioned raw materials, the degree of polymerization of PVA is 1500 ~ 3000, alcoholysis degree is 92 ~ 99mol%; Above-mentioned imvite is preferably at least one in sodium base, calcium base or magnesium base montmorillonite, fineness 1500 ~ 3000 order, if select two kinds of imvites, preferably adds according to 1: 1 ratio, selects that three kinds of imvites are then preferred to add by 1: 1: 1.
Find in the preparation process of PVA fiber, though the PVA fiber of medium modulus can be obtained as stated above, the easy conglomeration of imvite in preparation process, final PVA fiber modulus can be affected, PVA fiber quality is differed; In order to effectively prevent imvite conglomeration, make final obtained PVA fiber modulus homogeneous, above-mentioned raw materials also comprises 0.1 ~ 1 part of additive, is specially at least one in OP-10, TX-100 or carboxymethyl cellulose, is commercially available prod; If select two kinds of additives, preferably add according to 1: 1 ratio, select that three kinds of imvites are then preferred to add by 1: 1: 1.
Most preferably, the initial feed component that the preparation method of medium modulus PVA fiber of the present invention adopts is: the PVA of 100 parts, the imvite of 17 parts, the additive of 0.6 part and the deionized water of 650 ~ 680 parts; The wherein degree of polymerization 1500 ~ 3000 of PVA, alcoholysis degree is 92 ~ 99mol%, and imvite is fineness is 1500 ~ 3000 object sodium-based montmorillonites, and additive is TX-100.
Find further in R&D process, in above-mentioned mixed dissolution step, if control, bad easily to make PVA dissolve bad, thus affect spinning effect: shower nozzle easily blocks, easily breaks in wet spinning process, easily makes that the PVA fiber thickness that finally obtains is uneven, commercial quality is good not.In order to improve the quality homogeneity of final PVA fiber further, in above-mentioned raw materials mixed dissolution, mixing temperature is preferably 95 ~ 110 DEG C, and pressure is preferably 0.01 ~ 0.15MPa, and dissolution time is preferably 3 ~ 9 hours, is made into spinning solution; Be more preferably temperature 105 DEG C, pressure 0.08MPa, dissolution time 5 hours.
In order to improve spinning effect further, improve the intensity of final obtained PVA fiber, in above-mentioned wet spinning process, spinning head aperture is preferably 0.07 ~ 0.20mm, more preferably 0.1 ~ 0.12mm.
Specifically, a kind of preparation method of medium modulus PVA fiber, carries out as follows:
(1) preparation of spinning solution
Be 1500 ~ 3000 by the degree of polymerization, alcoholysis degree is the PVA100 weight portion of 92 ~ 99mol%, above-mentioned imvite 1 ~ 20 weight portion, above-mentioned additive 0.1 ~ 1 weight portion, deionized water 400 ~ 800 weight portion, add in dissolution kettle, under agitation in temperature 95 ~ 110 DEG C, pressure is 0.01 ~ 0.15MPa, dissolve 3 ~ 9 hours, be made into spinning solution, then by solution pressure filtration, deaeration, make spinning solution;
(2) wet spinning
Aperture is utilized to be 0.07 ~ 0.20mm wet spinning spinning head, by spinning solution in temperature 95 ~ 100 DEG C, through filter, measuring pump, spray from spinning head, stoste thread is shaping in the coagulating bath of stronger coagulation ability, adopt-0.5 ~ 1 times of spinneret draft, coagulating bath is 370 ~ 420g/l metabisulfite solution, and bath temperature is 35 ~ 60 DEG C;
(3) spinning post processing
A, drying: by 50 ~ 90wt% water that fiber contains, bake removing by multistage, and carry out preheating to fiber, make it to reach softening and be conducive to next step stretching;
B, stretching HEAT SETTING: heat setting temperature is 180 ~ 260 DEG C, hot-stretch 1 ~ 6 times, heat-setting time 3 ~ 10 minutes, obtains PVA fiber.
Preparation method of the present invention has following beneficial effect:
1, the present invention by add in PVA stoste imvite, all the other steps routinely wet spinning carry out, the fibrous physics mechanical performance obtained is increased dramatically, and especially Young's modulus has the increase of 30 ~ 100% compared with conventional wet lay spinning.
2, the present invention have employed auxiliary additive further in PVA stoste, and imvite is disperseed more even, stoste performance is more stable, is more conducive to spinning moulding, improves homogeneity and the quality of final obtained PVA fiber.
3, PVA fiber producing processes of the present invention is compared with high strength high modulus PVA fiber technique, simple to operate, with low cost, has more the feature of environmental protection, is particularly suitable for industrialization large-scale production.The PVA fiber linear density that the present invention obtains is 1.0 ~ 10.0dtex, dry fracture strength 6.0 ~ 10.0cN/dtex, extension at break 6 ~ 20%, Young's modulus 120 ~ 200cN/dtex; Be highly suitable in building field or industrial cloth and apply, its imvite adopted is natural minerals, in concrete mortar, more tight with the bonding of cement based.
Detailed description of the invention
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is; following examples are only for being further detailed the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to foregoing invention content to the present invention.
Embodiment 1
Be 1750 ± 50 by the degree of polymerization, alcoholysis degree is the PVA 15kg altogether of 95mol%, 1500 order calcium-base montmorillonite 0.3kg, OP-10 additive 0.1kg, water 84kg, join in dissolution kettle, under agitation in temperature 98 ± 2 DEG C, pressure 0.01MPa, dissolve after 4 hours, filter through transport pump, deaeration 18 hours under normal pressure, deaeration temperature 97 DEG C, obtained spinning solution temperature 97 DEG C, measured by measuring pump, via hole diameter is 0.10mm, the spinnerets spray silk in 6000 holes, solidification forming in saltcake coagulating bath, spinneret draft-0.5 times, spun as-spun fibre is through damp and hot, dry, stretch, HEAT SETTING, total stretching 6 times, obtained fiber linear density 3.1dtex, Young's modulus 118cN/dtex.
Embodiment 2
Be 1750 ± 50 by the degree of polymerization, alcoholysis degree is the PVA 15kg altogether of 99mol%, 1800 order sodium-based montmorillonite 0.3kg, TX-100 additive 0.2kg, water 84kg, join in dissolution kettle, under agitation in temperature 98 ± 2 DEG C, pressure 0.02MPa, dissolve after 3 hours, filter through transport pump, deaeration 4 hours under normal pressure, deaeration temperature 97 DEG C, obtained spinning solution temperature 97 DEG C, measured by measuring pump, via hole diameter is 0.10mm, the spinnerets spray silk in 6000 holes, solidification forming in saltcake coagulating bath, spinneret draft-0.2 times, spun as-spun fibre is through damp and hot, dry, stretch, HEAT SETTING, total stretching 9 times, obtained fiber linear density 2.2dtex, Young's modulus 160cN/dtex.
Embodiment 3
Be 1850 ± 50 by the degree of polymerization, alcoholysis degree is the PVA 15kg altogether of 99mol%, 3000 order sodium-based montmorillonite 0.6kg, TX-100 additive 0.2kg, water 85kg, join in dissolution kettle, under agitation in temperature 108 ± 2 DEG C, pressure 0.03MPa, dissolve after 6 hours, filter through transport pump, deaeration 16 hours under normal pressure, deaeration temperature 97 DEG C, obtained spinning solution temperature 97 DEG C, measured by measuring pump, via hole diameter is 0.08mm, the spinnerets spray silk in 8000 holes, solidification forming in saltcake coagulating bath, spinneret draft 0.1 times, spun as-spun fibre is through damp and hot, dry, stretch, HEAT SETTING, total stretching 9 times, obtained fiber linear density 1.8dtex, Young's modulus 198cN/dtex.
Embodiment 4
Be 2000 ± 50 by the degree of polymerization, alcoholysis degree is the PVA 14kg altogether of 99mol%, 2600 order magnesium base montmorillonite 0.3kg, OP-10 additive 0.1kg, water 86kg, join in dissolution kettle, under agitation in temperature 99 ± 1 DEG C, pressure 0.03MPa, dissolve after 6 hours, filter through transport pump, deaeration 16 hours under normal pressure, deaeration temperature 98 DEG C, obtained spinning solution temperature 98 DEG C, measured by measuring pump, via hole diameter is 0.10mm, the spinnerets spray silk in 6000 holes, solidification forming in saltcake coagulating bath, spinneret draft 0.9 times, spun as-spun fibre is through damp and hot, dry, stretch, HEAT SETTING, total stretching 9 times, obtained fiber linear density 2.1dtex, Young's modulus 190cN/dtex.
Comparative example 1
By PVA identical for embodiment 2 and solvent, not doping and imvite, fiber Young's modulus 110cN/dtex obtained under the same test conditions.
Embodiment 5 ~ 9
Undertaken by following material and technological parameter, other is all identical with embodiment 1.Obtained PVA fiber linear density is 1.0 ~ 10.0dtex, and dry fracture strength 6.0 ~ 10.0cN/dtex, extension at break 6 ~ 20%, Young's modulus 120 ~ 200cN/dtex, is highly suitable in building field or industrial cloth and applies.
Claims (12)
1. the preparation method of a medium modulus PVA fiber, first by raw material mixed dissolution, carry out conventional wet lay spinning again and obtain PVA fiber, it is characterized in that: described raw material comprises PVA, imvite and water, wherein PVA accounts for 100 parts, imvite accounts for 1 ~ 20 part, water accounts for 400 ~ 800 parts; Described imvite is at least one in sodium base, calcium base or magnesium base montmorillonite, fineness 1500 ~ 3000 order; In described raw material, the degree of polymerization of PVA is 1500 ~ 3000, alcoholysis degree is 92 ~ 99mol%.
2. preparation method as claimed in claim 1, is characterized in that: described each raw material is PVA 100 parts, imvite accounts for 17 parts, water accounts for 650 ~ 680 parts.
3. the preparation method as described in claim 2, is characterized in that: described raw material also comprises 0.1 ~ 1 part of additive, and described additive is at least one in OP-10, TX-100 or carboxymethyl cellulose.
4. preparation method as claimed in claim 1, is characterized in that: described raw material also comprises 0.1 ~ 1 part of additive, and described additive is at least one in OP-10, TX-100 or carboxymethyl cellulose.
5. preparation method as claimed in claim 4, is characterized in that: described raw material components is: the PVA of 100 parts, the imvite of 17 parts, the additive of 0.6 part and the deionized water of 650 ~ 680 parts; The wherein degree of polymerization 1500 ~ 3000 of PVA, alcoholysis degree is 92 ~ 99mol%, and imvite is fineness is 1500 ~ 3000 object sodium-based montmorillonites, and additive is TX-100.
6. preparation method as claimed in claim 3, it is characterized in that: in described raw material mixed dissolution, mixing temperature is 95 ~ 110 DEG C, and pressure is 0.01 ~ 0.15MPa, and dissolution time is 3 ~ 9 hours, is made into spinning solution.
7. preparation method as claimed in claim 6, it is characterized in that: in described raw material mixed dissolution, mixing temperature is 105 DEG C, and pressure is 0.08MPa, and dissolution time is 5 hours.
8. preparation method as claimed in claim 5, it is characterized in that: in described raw material mixed dissolution, mixing temperature is 95 ~ 110 DEG C, and pressure is 0.01 ~ 0.15MPa, and dissolution time is 3 ~ 9 hours, is made into spinning solution.
9. preparation method as claimed in claim 8, it is characterized in that: in described raw material mixed dissolution, mixing temperature is 105 DEG C, and pressure is 0.08MPa, and dissolution time is 5 hours.
10. the preparation method as described in claim 3 or 5, is characterized in that: in described wet spinning process, and spinning head aperture is 0.07 ~ 0.20mm.
11. preparation methods as claimed in claim 10, it is characterized in that: in described wet spinning process, spinning head aperture is 0.1 ~ 0.12mm.
12. preparation methods as claimed in claim 4, carry out as follows:
(1) preparation of spinning solution
Add in dissolution kettle by described PVA, imvite, additive and deionized water, under agitation in temperature 95 ~ 110 DEG C, pressure is 0.01 ~ 0.15MPa, dissolves 3 ~ 9 hours, is made into spinning solution, then by solution pressure filtration, deaeration, makes spinning solution;
(2) wet spinning
Aperture is utilized to be 0.07 ~ 0.20mm wet spinning spinning head, by spinning solution in temperature 95 ~ 100 DEG C, through filter, measuring pump, spray from spinning head, stoste thread is shaping in the coagulating bath of stronger coagulation ability, adopt-0.5 ~ 1 times of spinneret draft, coagulating bath is 370 ~ 420g/L metabisulfite solution, and bath temperature is 35 ~ 60 DEG C;
(3) spinning post processing
A, drying: by 50 ~ 90wt% water that fiber contains, bake removing by multistage, and carry out preheating to fiber, make it to reach softening and be conducive to next step stretching;
B, stretching HEAT SETTING: heat setting temperature is 180 ~ 260 DEG C, hot-stretch 1 ~ 6 times, heat-setting time 3 ~ 10 minutes, obtains PVA fiber.
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| CN104963022B (en) * | 2015-07-07 | 2017-06-27 | 中国科学院重庆绿色智能技术研究院 | The preparation method and product of a kind of high strength and modulus polyvinyl alcohol graphene quantum dot composite fibre |
| CN106637468A (en) * | 2016-12-09 | 2017-05-10 | 南通博泰美术图案设计有限公司 | Polyvinyl alcohol monofilament and production method thereof |
| CN111051584A (en) * | 2017-09-08 | 2020-04-21 | 株式会社可乐丽 | Polyvinyl alcohol fiber |
| CN111101218A (en) * | 2018-10-26 | 2020-05-05 | 中国石油化工股份有限公司 | High-strength polyvinyl alcohol fiber for yarn and preparation method and application thereof |
| CN109853070B (en) * | 2019-02-28 | 2021-06-15 | 陕西师范大学 | Montmorillonite/polyvinyl alcohol composite flame-retardant fiber |
| CN114182363B (en) * | 2020-10-12 | 2022-10-14 | 青岛尼希米生物科技有限公司 | Cellulose fiber capable of adsorbing and quickly deeply dyeing and preparation method and application thereof |
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| CN1197858A (en) * | 1998-04-14 | 1998-11-04 | 中国石油化工总公司 | Wet PVA-crosslinking spinning technology |
| CN102031571A (en) * | 2009-09-30 | 2011-04-27 | 中国石油化工集团公司 | Preparation method and application of water-soluble polyvinyl alcohol short fibers |
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