CN1403641A - Water soluble polyvinyl alcohol fiber and its prepn and use - Google Patents
Water soluble polyvinyl alcohol fiber and its prepn and use Download PDFInfo
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- CN1403641A CN1403641A CN 02133903 CN02133903A CN1403641A CN 1403641 A CN1403641 A CN 1403641A CN 02133903 CN02133903 CN 02133903 CN 02133903 A CN02133903 A CN 02133903A CN 1403641 A CN1403641 A CN 1403641A
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Abstract
The present invention features that PVA of polymerization degree 500-2000 and alcoholysis degree 75-99 mol% in 100 portions is mixed with solvent mixture of dimethyl sulfoxide and water in 200-400 portions, the mixture is stirred and heated to 80-120 deg.c at -0.01--0.08 MPa pressure in a stainless steel reactor for 3-4 hr to compound the spinning solution, and the spinning solution is filtered and defoamed and used in spinning to obtain water soluble PVA fiber after post-treatment. The PVA fiber has a water solving temperature of 10-90 deg.c, strength greater than 3.5 cN/dtex, monofilament length of 1.5-10 dtex, fracture elongation of 15-30%. It may be processed into top, which may further blended with wool top, cotton, top, etc. to produce fine yarn or hollow yarn, or cut into staple fiber for producing non-woven fabric, etc.
Description
One, technical field
The present invention relates to a kind of dimethyl sulfoxide (DMSO)/water mixed solvent with the dissolving of the polyvinyl alcohol blend of different polymerization degree, different alcoholysis degrees, be made into spinning solution with viscosity higher, by dry-wet spinning, extraction, drying, drawing and setting, obtain water-soluble polyvinyl alcohol fibers.
Two, background technology
Polyvinyl alcohol contains great amount of hydroxy group, has good water-solubility, it is higher particularly to work as acetoxy group content, big molecule regularity is poor, the possibility of crystallization is little, the characteristic of good water solubility, therefore by different polymerization degree, the fiber of the different water solution temperatures of spinning is feasible behind the polyvinyl alcohol blending of different alcoholysis degrees.
The method of making the polyvinyl alcohol water soluble fiber mainly contains water system wet spinning, dry spinning, wet method gel spinning and dried wet method gel spinning.Present domestic employing water system wet spinning can obtain 90 ℃ of water solution temperatures, dry strength 4.0cN/dtex, the polyvinyl alcohol water soluble fiber of stem elongation 30 ± 5% (Development and Production " polyvinyl communication " the 3rd phase in 1996 of the big peak of fourth soluble vinylon fiber).The water soluble fiber section that is obtained by this method is a kidney shape, is difficult to be not with the water-soluble fiber of low temperature of salt, behind the desalination, sticks together easily during fiber drying in process of production, and application is brought adverse effect.
Japanese patent gazette 8992/1968 adopts dry spinning to obtain water-soluble fibre, shrinkage factor height (30%) when this fiber dissolves in water, and this fiber and other fiber blend spin or make penelope, make embroidered pattern or fabric distortion when water-soluble.
The less fiber of shrinkage factor when the polyvinyl alcohol with low degree of polymerization spinning that Japanese special permission discloses 28408/1987 disclosure makes water-soluble, this method is with polyvinyl alcohol of high degree of polymerization and polyvinyl alcohol with low degree of polymerization co-blended spinning, make the polyvinyl alcohol water-soluble fibre that shrinkage factor is not more than 20%, intensity is not more than 2.65cN/dtex, such lower tenacity fibers processability in woven, knitting, bonded fabric process is relatively poor, easily broken end and damaged.
Japan's special permission discloses the 229805/1989 high-strength water-soluble polyvinyl alcohol fibers of introducing, it is that partly-hydrolysed polyvinyl alcohol is dissolved in the dimethyl sulfoxide (DMSO), dry-jet wet-spinning in the methyl alcohol solidification liquid, with high draw ratio cured fiber is carried out drawing-off after, obtain water-soluble polyvinyl alcohol fibers.This fiber has bigger contraction when depositing under high humility because of it, and the fiber size poor stability is owing to not providing good DIMENSIONAL STABILITY to limit its range of application.
The poly-vinyl alcohol solution of the organic solvent dissolution of Chinese patent 94108628.3 reports is through dry-jet wet-spinning or wet spinning, extraction stretching, multistage hyperthermic treatment and contraction, the water solution temperature of its fiber is not more than 100 ℃, shrinkage factor is not more than 20% in the water, the low temperature water soluble fiber adopts polyvinyl alcohol with low alcoholysis level, the high temperature water soluble fiber adopts high alcoholysis degree polyvinyl alcohol to make raw material, spins the water soluble fiber of different temperatures respectively.What adopt is organic solvent entirely, and dissolution time is long, and by highly stretch, the high contraction realize low contraction when water-soluble, water solution temperature is low more, intensity is low more, application is restricted.
Three, summary of the invention
The objective of the invention is provides a kind of water-soluble polyvinyl alcohol fibers and dry-wet spinning thereof at the deficiencies in the prior art, be characterized in adopting dimethyl sulfoxide (DMSO)/water mixed solvent, make the polyvinyl alcohol dissolution time short, dissolving fully, the solution good spinnability is by dry-wet spinning production high quality water soluble fiber.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The recipe ingredient of water-soluble polyvinyl alcohol fibers initiation material is:
The polyvinyl alcohol degree of polymerization 500～2000
100 parts of alcoholysis degree 75～99mol%
Solvent dimethyl sulfoxide (DMSO)/H
2O=90～70: 10～30 200～400 part
The vinal section of producing is circular, 10～90 ℃ of water solution temperatures, intensity 〉=3.5cN/dtex, filament fiber number 1.5～10dtex, extension at break 15～30%.
The dried wet process of water-soluble polyvinyl alcohol fibers
1, the preparation of spinning solution is with the degree of polymerization 500～2000,100 parts of the polyvinyl alcohol of alcoholysis degree 75～99mol%, dimethyl sulfoxide (DMSO)/water=95～70: 10～30 200～400 parts, join in the stainless steel dissolution kettle, under agitation in 80～120 ℃ of temperature, pressure-0.01～-0.08MPa dissolving 3-4 hour, be made into spinning solution, again with solution pressure filtration, deaeration, make spinning solution.
2, dry-wet spinning
Utilize special-purpose spinning head, aperture 0.08～0.2mm, with spinning solution in 80～120 ℃ of temperature, spray from spinning head through measuring pump, dynamic analysis of spinning is in viscous state in the air gap between spinnerets and coagulating bath, enter coagulating bath after 1～20 times of the spinneret draft, coagulating bath is a methyl alcohol, dimethyl sulfoxide (DMSO) and water content are not higher than 10% in the bath, and bathing temperature is-18～5 ℃, and just the as-spun fibre that forms is a gel state, still has bigger deformability, by the spinning super drawing, the fibre diameter after the stretching is less, helps extraction and post processing.
3, spinning post processing
(1) extraction: extraction adopts the outlet of counter-current, fiber to enter extractant methyl alcohol, and fiber is 5～30 ℃ of temperature in the extraction process, and by the extraction switch, 3～5 minutes time, 1～3 times of drawing-off simultaneously contains dimethyl sulfoxide (DMSO)≤0.1% in the fiber.
(2) oil: adopt the alcohol-soluble printing agent to eliminate static, increase fibre cohesion, avoid fiber to stick together when dry and typing, it is good to open fibre, helps weaving processing.
(3) drying: with the methyl alcohol that contains 50～100% on the fiber, remove by baking, fiber bakes under tense situation, adopts hot N
2Heating, methyl alcohol is reclaimed in the condenser cooling.
(4) hot-stretch typing: heat setting temperature is 120～240 ℃, 2～5 times of hot-stretchs, heat-setting time 1～8 minute, percent thermal shrinkage 5～30%, 10～90 ℃ of the water solution temperatures of acquisition fiber.
The dry-wet spinning that the present invention adopts, from the post processing that is prepared into of spinning solution, overall process is airtight fully, and solvent, coagulating agent and extractant reclaim entirely, and no emission is the fiber production method of environment-friendly type.The fiber section of producing is circular, moisture regain back fiber does not shrink dimensionally stable, fibre strength 〉=3.5cN/dtex, extension at break 15～30%, 10～90 ℃ of water solution temperatures, shrinkage factor is less, and the ash content of coal is less than 1%, this water-soluble fibre can be produced long filament or be processed into wool top, with wool tops, sliver, fiber crops and chemical fibre blending, make high grade yarn or hollow yarn, staple fibre is made the multiple use of nonwoven fabric, penelope and papermaking aspect.
The present invention has following advantage:
1, adopt dimethyl sulfoxide (DMSO)/water mixed solvent, the polyvinyl alcohol dissolution time shortened more than 2/3, dissolving fully, the gel-free particle, good spinnability, spinning changes that a rate is low, lousiness is few, also can reduce solvent cost.
2, dry-wet spinning can carry out super drawing at spinning head, and it is less to obtain single fiber diameter, helps the extraction and the post processing of solvent.The distance of air layer can be regulated between spinning head and the solidification liquid, guarantees that thread is in the time of viscosity flow state.
3, adopt the polyvinyl alcohol blending spinning of different polymerization degree, different alcoholysis degrees, make full use of polyvinyl alcohol structures, the performance characteristics of different size, the processability excellence, satisfy the water-soluble polyvinyl alcohol fibers of multiple requirement.
4, the polyvinyl alcohol degree of polymerization or alcoholysis degree difference, its performance difference is very big, the degree of polymerization 〉=1700 for example, the polyvinyl alcohol of alcoholysis degree 〉=99% will dissolve more than 5 hours in the water more than 90 ℃, could dissolve fully; And the same degree of polymerization, alcoholysis degree are the polyvinyl alcohol of 88～90mol%, just can dissolve at 30 ℃; The degree of polymerization 1000, the polyvinyl alcohol of alcoholysis degree 99mol% just can dissolve in the time of 80 ℃ fully; The degree of polymerization and alcoholysis degree are low, solution temperature is low, can spin the lower fiber of water solution temperature, but the fiber size instability, moisture regain easily, fiber shrinks, and intensity is low, therefore, the specification that chooses polyvinyl alcohol is to produce one of the key technology of the water-soluble fibre of excellent performance.
5, adopt the poly-ethanol spinning water soluble fiber of the different alcoholysis degrees of different polymerization degree, high polymerization degree, high alcoholysis degree polyvinyl alcohol play skeleton function in fiber, for fiber provide higher intensity, low polymerization degree, polyvinyl alcohol with low alcoholysis level make fiber have dissolution velocity fast, dissolve characteristic completely.
Four, the specific embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; 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 to the present invention according to the invention described above content.
Embodiment 1
With the degree of polymerization 1750 ± 50, the polyvinyl alcohol 19.6kg of alcoholysis degree 97mol% and the degree of polymerization 1750 ± 50, the polyvinyl alcohol 8.4kg blend of alcoholysis degree 92mol% adds in the stainless steel dissolution kettle of dimethyl sulfoxide (DMSO)/water=90/10 72kg, under agitation in 100 ± 3 ℃ of temperature, pressure-0.05Mpa, dissolve after 3 hours, filter normal pressure deaeration 10 hours, 97 ℃ of deaeration temperature through pump pressure, make 97 ℃ of spinning solution temperature, by measuring pump, via hole diameter is 0.15mm, the spinnerets ejection in 500 holes, in the methyl alcohol coagulating bath through air gap and-8 ℃, 8 times of spinneret drafts, spun as-spun fibre be wet the stretching 2 times in 25 ℃ of methanol bath, makes wet drawing of fiber drawing extraction in methanol bath remove dimethyl sulfoxide (DMSO) again, the extraction time is 5 minutes, oils, tow is at 120 ℃ N
2Dry in the gas tank, then, through 120 ℃, 180 ℃, 200 ℃ hot-stretch typings, make 78～83 ℃ of water solution temperatures, line density is the polyvinyl alcohol filaments of 1000dtex, dimethyl sulfoxide (DMSO) content≤0.1%, fracture strength 5.0cN/dtex, extension at break 13～20%, fiber surface is smooth, and section is circular.
Comparative Examples 1, the polyvinyl alcohol that embodiment 1 is identical adopts absolute dimethyl sulfoxide to make solvent, dissolves under the same process condition, and dissolution time is after 6.5 hours, and micelle just disappears substantially.
Comparative Examples 2 is by the process conditions of implementing 1, only with the degree of polymerization 1750 ± 50, the polyvinyl alcohol of alcoholysis degree 97mol%, spinning solution concentration 29%, fiber are when the stretching HEAT SETTING, during 120～200 ℃ of temperature, water solution temperature is 50 ℃, temperature is when 180～200 ℃ of drawing and settings, and water solution temperature is 84 ℃, and water solution temperature alters a great deal with the typing condition; After sneaking into the lower polyvinyl alcohol of alcoholysis degree, its water solution temperature changes little with the typing condition, the easier control of process conditions.
Embodiment 2
With the degree of polymerization 1000 ± 50, the polyvinyl alcohol 19.5kg of alcoholysis degree 99mol% and the degree of polymerization 1750 ± 50, the polyvinyl alcohol 10.5kg blend adding of alcoholysis degree 88mol% fills in the stainless steel dissolution kettle of dimethyl sulfoxide (DMSO)/water=90/10 70kg, under agitation in 100 ± 3 ℃ of temperature, pressure-0.02MPa dissolved 3.5 hours, filter through pump pressure, normal pressure deaeration 10 hours, 97 ℃ of deaeration temperature, obtain the few spinning solution of colloidal particle at last, 97 ℃ of this spinning solution temperature are passed through measuring pump, aperture 0.20mm, the spinnerets ejection in 500 holes, from solidification liquid air gap height 25mm, solidification liquid methyl alcohol/dimethyl sulfoxide (DMSO)=95: 5,10 times of spinneret drafts stretch 1.8 times in 20 ℃ methanol bath, reverse extraction is 5 minutes in the methanol bath that the extraction switch is housed, and fiber is at the N of 125～127 ℃ of temperature behind the press for extracting juice liquid
2Drying is removed methyl alcohol in the gas, handles at 130～210 ℃ of drawing and settings of temperature, obtains fibre strength 4.8cN/dtex, filament fiber number 2dtex, extension at break 18～23%, 52 ℃ of water solution temperatures.
Comparative Examples 3
Press the spinning solution and the spinning technique of embodiment 2 preparations, selecting the spinneret draft multiple is 1, strengthens the after-drawing multiple, can only obtain the fiber of filament 〉=5dtex, can not obtain the water-soluble polyvinyl alcohol fibers of filament fiber number 2dtex.
Comparative Examples 4
Be prepared as spinning solution by embodiment 2, spinning technique, do not adopt the extraction switch when selections are got, dimethyl sulfoxide (DMSO) content is 5% in the fiber, and adopts the extraction switch, dimethyl sulfoxide (DMSO) content≤0.1% in the fiber of extraction back.
Embodiment 3
With the degree of polymerization 1750 ± 50, the polyvinyl alcohol 16.5kg of alcoholysis degree 95mol% and the degree of polymerization 500 ± 50, the polyvinyl alcohol 14kg blend of alcoholysis degree 88mol%, add and fill in the stainless steel dissolution kettle of dimethyl sulfoxide (DMSO)/water=92/8 69.5kg, under agitation in 97 ℃ of temperature, pressure-0.01Mpa dissolved 3.5 hours, filter through pump pressure, normal pressure deaeration 10 hours makes the former source of spinning, and this spinning solution passes through measuring pump for 97 ℃ in temperature, via hole diameter 0.2mm, the spinnerets ejection in 500 holes, spin in-8 ℃ the methyl alcohol coagulating bath, 10 times of spinneret drafts stretch 2 times in 30 ℃ of methanol bath, reverse extraction is 3 minutes in the methanol bath that the hydraulic fluid device is housed, oil, dry, the hot-stretch typing is with implementing 1, and the acquisition water solution temperature is 22 ℃ a vinal, intensity 3.6cN/dtex, extension at break 20-26%, section is circular, no core-skin layer structure, smooth surface.
Claims (3)
1, the recipe ingredient of water-soluble polyvinyl alcohol fibers initiation material (by weight) is
The degree of polymerization 500～2000,100 parts of the polyvinyl alcohol of alcoholysis degree 75～99mol%, solvent dimethyl sulfoxide (DMSO)/water=90～70: 10～30 200～400 parts
The main performance of water-soluble polyvinyl alcohol fibers:
Section is 10～90 ℃ of circles, smooth surface, water solution temperature, intensity 〉=3.5cN/dtex, filament fiber number 1.5～10dtex, extension at break 15～30%.
2, according to the preparation method of the described water-soluble polyvinyl alcohol fibers of claim 1, it is characterized in that:
(1) preparation of spinning solution
With the degree of polymerization 500～2000,100 parts of the polyvinyl alcohol of alcoholysis degree 75～99mol%, dimethyl sulfoxide (DMSO)/water=95～70: 10～30 200～400 parts, join in the stainless steel dissolution kettle, under agitation in 80～120 ℃ of temperature, pressure-0.01～-0.08MPa dissolving 3～4 hours, wiring solution-forming, again with solution pressure filtration, deaeration, make spinning solution
(2) dry-wet spinning
Utilize special-purpose spinning head, aperture 0.08～0.2mm, spinning solution is sprayed from spinning head in 80～120 ℃ of processes of temperature measuring pump, dynamic analysis of spinning is in viscous state in the air gap between spinnerets and coagulating bath, enter coagulating bath after 1～20 times of the spinneret draft, coagulating bath is a methyl alcohol, dimethyl sulfoxide (DMSO) and water content are not higher than 10% in the bath, bathing temperature is-18～5 ℃, and just the as-spun fibre that forms is a gel state, still has bigger deformability, by the spinning super drawing, fibre diameter after the stretching is less, helps extraction and post processing
(3) spinning post processing
A, extraction: extraction adopts the outlet of counter-current, fiber to enter extractant methyl alcohol, and fiber is 5～30 ℃ of temperature in the extraction process, and by the extraction switch, 3～5 minutes time, 1～3 times of drawing-off simultaneously contains dimethyl sulfoxide (DMSO)≤0.1% in the fiber,
B, oil: adopt the alcohol-soluble printing agent to eliminate static, increase fibre cohesion, avoid fiber to stick together when dry and typing, it is good to open fibre, helps weaving processing,
C, drying: with the methyl alcohol that contains 50～100% on the fiber, remove by baking, fiber bakes under tense situation, adopts hot N
2Heating, methyl alcohol is reclaimed in the condenser cooling,
D, hot-stretch typing: heat setting temperature is 120～240 ℃, 2～5 times of hot-stretchs, heat-setting time 1～8 minute, percent thermal shrinkage 5～30%, 10～90 ℃ of the water solution temperatures of acquisition fiber.
3, according to the purposes of claim 1 or 2 described water-soluble polyvinyl alcohol fibers, it is characterized in that this fiber can produce long filament or be processed into wool top, make high grade yarn or hollow yarn with wool tops, sliver, fiber crops and chemical fibre blending, staple fibre is made the multiple use of nonwoven fabric, penelope and papermaking aspect.
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| CN 02133903 CN1253616C (en) | 2002-10-14 | 2002-10-14 | Water soluble polyvinyl alcohol fiber and its prepn and use |
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| CN100339519C (en) * | 2005-12-13 | 2007-09-26 | 中国石化集团四川维尼纶厂 | Method of preparing high performance polyvinyl alcohel fiber |
| CN101177800B (en) * | 2006-11-06 | 2010-08-11 | 湖南省湘维有限公司 | Water-soluble polyvinyl alcohol fibre and preparation technique thereof |
| CN102031572A (en) * | 2009-09-30 | 2011-04-27 | 中国石油化工集团公司 | Preparation technique of water-soluble polyvinyl alcohol fiber and application thereof |
| CN101747459B (en) * | 2008-12-02 | 2011-09-07 | 卢金永 | Preparation method of dispersing agent of chemically modified polyvinyl alcohol |
| CN102493014A (en) * | 2011-11-15 | 2012-06-13 | 天津科技大学 | Epsilon-polylysine and polyvinyl alcohol composite biological antibacterial fiber and preparation method thereof |
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| CN108754640A (en) * | 2018-06-07 | 2018-11-06 | 江苏广盛源科技发展有限公司 | A kind of automatic intelligent special fibre spinning-drawing machine |
| CN109208146A (en) * | 2017-07-05 | 2019-01-15 | 上海水星家用纺织品股份有限公司 | The method for weaving of cotton and the blended hollow yarn man textile fabric of polyvinyl |
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- 2002-10-14 CN CN 02133903 patent/CN1253616C/en not_active Expired - Lifetime
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| CN101177800B (en) * | 2006-11-06 | 2010-08-11 | 湖南省湘维有限公司 | Water-soluble polyvinyl alcohol fibre and preparation technique thereof |
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| CN102031572B (en) * | 2009-09-30 | 2015-08-05 | 中国石油化工集团公司 | A kind of preparation technology of water-soluble polyvinyl alcohol fibers and application thereof |
| CN102031572A (en) * | 2009-09-30 | 2011-04-27 | 中国石油化工集团公司 | Preparation technique of water-soluble polyvinyl alcohol fiber and application thereof |
| CN102912471A (en) * | 2011-08-04 | 2013-02-06 | 中国石油化工集团公司 | 70 DEG C water-soluble polyvinyl alcohol fiber with small dissolution range and preparation method thereof |
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| CN102493014B (en) * | 2011-11-15 | 2016-03-30 | 天津科技大学 | A kind of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre and preparation method thereof |
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| CN102731708A (en) * | 2012-06-13 | 2012-10-17 | 安徽皖维集团有限责任公司 | Preparation method of polyvinyl alcohol with high alcoholysis degree |
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| CN109208146A (en) * | 2017-07-05 | 2019-01-15 | 上海水星家用纺织品股份有限公司 | The method for weaving of cotton and the blended hollow yarn man textile fabric of polyvinyl |
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| CN115992396A (en) * | 2021-10-20 | 2023-04-21 | 中国石油化工股份有限公司 | Application of reducing acidity of oil bath in improving whiteness of fiber |
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