CN101177800A - Water-soluble polyvinyl alcohol fibre and preparation technique thereof - Google Patents
Water-soluble polyvinyl alcohol fibre and preparation technique thereof Download PDFInfo
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Abstract
The invention relates to a water-soluble polyvinyl alcohol fiber and a preparation method thereof. The water-soluble polyvinyl alcohol fibers provided by the invention has the following natural parameters: the dry breaking strength of fibers is more than or equal to 5cN/dtex; dry breaking elongation rate is 10 percent to 20 percent; water solution temperature is 60 DEG C to 90 DEG C; single fiber titer is 1.0dtex to 8dtex; the number of crimp is 8 to 12/25mm. The invention conquers the imperfections of the existing method of long technique procedure and high production energy consumption caused by the redrying of fibers, furthermore, the property of the prepared water-soluble polyvinyl alcohol fibers is improved to some extent.
Description
Technical field
The present invention relates to a kind of water-soluble polyvinyl alcohol fibers.The invention still further relates to the preparation technology of this water-soluble polyvinyl alcohol fibers, particularly the water system wet spinning technology.
Background technology
The mean molecule quantity of the raw materials used polyvinyl alcohol of vinal is 60000～150000, and heat decomposition temperature is 200～220 ℃, and fusing point is 225～230 ℃.Vinal can make with wet spinning and dry spinning.
Water-soluble polyvinyl alcohol fibers is a kind of of polyvinyl fibre in differentiation.Japan is the country that develops water soluble fiber the earliest.Water-soluble polyvinyl alcohol fibers can be produced (Li Shenglin by technologies such as conventional wet spinning process, organic solvent wet spinning, dry-wet spinning, dry spinning, the spinning of semi-molten method, Qin Feng, water-soluble polyvinyl alcohol fibers and polyvinyl alcohol dry spinning, the polyvinyl communication, 2004,24 (4): 7-11).Domestic basic employing water system wet spinning can obtain 90～94 ℃ of water solution temperatures at present, does fracture strength 4.0cN/dtex, the polyvinyl alcohol water-soluble fibre of dried elongation at break 30 ± 5%.Its technological process is: 1, the preparation process of spinning solution is: with the degree of polymerization 800～2000,100 parts of the polyvinyl alcohol of alcoholysis degree 88～99mol% are after washing, purify waste water with 400～600 parts and to join in the dissolution kettle, under agitation in 98 ± 2 ℃ of temperature, pressure-0.01～-0.03Mpa dissolving 3～4 hours, then solution pressure filtration, deaeration are mixed with spinning solution; 2, the wet spinning process is: (the spinning head specification: 24000～30000 holes, aperture 0.05～0.1mm), dynamic analysis of spinning is approaching saturated saltcake (Na from the spinning head ejection through measuring pump with spinning solution (98 ± 2 ℃ of temperature) to utilize power
2SO
4) be frozen into as-spun fibre (bathing 42～46 ℃ of temperature) in the coagulating bath, through deflector roll stretch and damp and hot stretching after enter heat treatment process; 3, heat treatment process: fiber carries out drying by Electric heat oven under tense situation, implements xeothermic stretching, HEAT SETTING after preheating, and silk axle car is shunk, is wound in cooling then, cuts off the back with sending cotton blower fan to deliver to finishing process; 4, spinning post processing: from sending fiber that cotton blower fan comes, carry out that hot water curls, the normal temperature washing, oil, after opening fibre, enter drier, be packaged into product at last by the arrangement acetalizing machine.
Above-mentioned existing method technological process is long, and fiber is through redrying, energy consumption height; Arrangement acetalizing machine and drying machine are large-scale and complicated device, and maintenance difficulty is big, makes product contain impurity such as yellow cotton, dirty cotton, influences product quality; And fiber contains a small amount of salinity in the production process, is difficult to obtain the water-soluble fiber of low temperature, can not satisfy user's multiple demand.
When said method was produced 90 ℃ of water soluble fibers, the characterisitic parameter of water-soluble polyvinyl alcohol fibers is as follows: dried fracture strength was 3.0～4.5cN/dtex; Dried elongation at break, 27 ± 7%; Molten disconnected temperature, 91～94 ℃; Crispation number, 3.2～4.5/25mm.
Chinese patent application prospectus (application number 94103580.8) has been announced the wet process technique of water-soluble fibre, and technical process is: the dissolving of material polyethylene alcohol, stoste modification, once filtration, deaeration, secondary filter, spinning, heat treatment, cut-out, post processing (comprise washing, oil, drying), pack.This method belongs to traditional wet spinning technology, it is characterized in that the polyvinyl alcohol of the degree of polymerization about 1800 is carried out degradation treatment by chemical method, obtains the stoste degree of polymerization 800～1100, thereby makes 75～90 ℃ water-soluble polyvinyl alcohol fibers.
The coiling method of fiber has machine crimp, hot water to curl and hot blast curls three kinds.The hot water technology of curling is all adopted in the wet spinning production of present domestic water-soluble polyvinyl alcohol fibers, and the back fiber crimp number that curls has only 3～5/25mm.Bibliographical information, the dry method of water-soluble poval and dry-wet spinning method all adopt the hot blast technology of curling, and it is to utilize the internal strain of fiber to take place to curl, and its crispation number is improved to some extent than hot water is curling, but uniformity is not so good.
Machine crimp technology is widely used in other fiber production process such as terylene, aramid fiber at present, its curling process conditions are wet volume, hot rolling, be that fiber carried out heat treated by hot water storgae before entering the machine crimp machine, fiber contains a large amount of moisture content in curly course, curling temperature is 100～120 ℃.
The method that oils of fiber is divided into substantially that oil bath oils and the machinery two big classes that oil, and machinery oils and can be divided into that surface contact oils and two kinds of oil spouts.The mode that oils of present domestic conventional vinylon fiber and water-soluble polyvinyl alcohol fibers all adopts oil bath to oil, and the rate of oiling is controlled at about 0.4%, 30～40 ℃ of oil bath temperatures.
Present mechanical oiling process is widely used in the fiber production process such as terylene, polypropylene fibre and acrylic fibers, its principle: with the many group roller (surface of roller be immersed in oil groove) of fiber by oiling machine, thereby reach the purpose that fiber surface oils, or oiling machine be equipped with several to nozzle, thereby with the fiber surface that vaporific form is sprayed onto by oiling machine tow is oiled oil.
Summary of the invention
Water-soluble polyvinyl alcohol fibers preparation technology of the present invention comprises following process: the preparation of spinning solution, wet spinning, heat treatment process and spinning post processing, wherein
Heat treatment process is:
(1) washing: adopt the adverse current WATER-WASHING METHOD, fiber and soft water counter current contacting in rinsing bowl, washing temperature are controlled at 20～40 ℃, and fiber is saltcake adhesive rate≤1% after washing;
(2) preliminary treatment: adopt high-temperature resistant water dissolubility finish that fiber is carried out preliminary treatment, make fiber reach the technological requirement of heat treatment process;
(3) drying: 60～70% moisture content that contain on the fiber are removed;
(4) xeothermic stretching, typing: dried fiber is implemented xeothermic stretching after preheating, and carry out HEAT SETTING then and handle, 1～2 times of xeothermic stretching, heat setting temperature is 220～280 ℃, heat-setting time 1～5 minute;
The spinning last handling process is:
(1) oil: fiber oils by oiling machine;
(2) curl: adopt machine crimp technology.Fiber oils after smooth preliminary treatment is carried out machine crimp by the machine crimp machine.
In the above-mentioned drying process, fiber carries out drying under tense situation.
The finish adhesive rate can be regulated as required.
Can regulate the fiber crimp number by the parameters of adjusting crimping machine.
The present invention adopts and optimizes improved wet spinning production technology, does not shrink dimensionally stable after the fiber moisture regain of production, fiber is done fracture strength 〉=5cN/dtex, dried elongation at break 10～20%, 60～90 ℃ of water solution temperatures, filament fiber number 1.0～8dtex, 8～12/25mm of crispation number.
With same raw material, adopt technology existing and provided by the invention to produce water-soluble fibre, the parameter comparison of the fiber that is obtained sees the following form.
| Sequence number | Project | Index | Old technology | New technology |
| 1 | Do fracture strength, cN/dtex 〉= | 3.2 | 3.0～4.5 | 5.0 |
| 2 | Dried elongation at break, % | 27±7 | 27±7 | 10～20 |
| 3 | Molten disconnected temperature, ℃≤ | 94.0 | 91～94 | 85～90 |
| 4 | Crispation number, individual/25mm 〉= | 3.0 | 3.2～4.5 | 8～12 (can regulate) |
| 5 | The rate that oils, % | 0.4 | 0.4 | Regulate as required |
This water-soluble fibre can the production endless tow or is processed into wool top, with wool, sliver, fiber crops and chemical fibre blending, makes high grade yarn or hollow yarn, or cuts into the multiple use that staple fibre is made aspects such as nonwoven fabric, penelope and papermaking.
The present invention has the following advantages:
1, the optimization and the shortening technological process of production on conventional wet spinning basis become primary drying with redrying, and fiber can the loss-rate conventional wet descend 30～40%, and manufacturing cost descends 800～1000 yuan/ton.
2, adopt machine crimp to substitute the warm water technology of curling, make the curling number of fiber bring up to 8～12/25mm, and the number of can flexible modulation curling, can satisfy the needs of the different purposes of user from 3～4/25mm.
3, adopt mechanical oiling process, but fibre finishing adhesive rate flexible modulation makes the fibre spinnable silk better, can satisfy the needs of the different purposes of user.
4, the production technology after employing improves, the gained quality of fiber is better, is raw material with specification polyvinyl alcohol of the same race, and fibre strength is higher, shrinkage factor is littler, water solution temperature is lower, and does not have impurity such as assorted cotton, dirty cotton.
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 foregoing invention content.
Embodiment 1
With the degree of polymerization 1750 ± 80, the polyvinyl alcohol 32kg of alcoholysis degree 99mol% is after washing, add in the dissolution kettle with purifying waste water of 168kg, under agitation in 98 ± 2 ℃ of temperature, pressure-0.015Mpa, dissolve after 3.5 hours, after filtration, normal pressure discontinuous degassing 6～8 hours makes spinning solution 98 ± 0.5 ℃ of temperature, after the measuring pump metering, by aperture 0.07mm, the spinning head ejection in 30000 holes is frozen into as-spun fibre in 44 ± 1 ℃ saltcake are bathed, stretch 2.5 times through deflector roll, 1.6 times of damp and hot stretchings, tow is by demineralized water tank flush away saltcake, enters in 220～250 ℃ the baking oven dryly after preliminary treatment, passes through preheating then, 220～280 ℃ of xeothermic stretchings and HEAT SETTING, dried 1.3 times of the multiples that draw, oil through machinery again, machine crimp, the dried fracture strength that makes water-soluble fibre is 7.5cN/dtex, single fiber line density 1.1dtex, dried elongation at break 10～16%, 85～90 ℃ of water solution temperatures.
The comparative example 1, is raw material with the same size polyvinyl alcohol, adopts the conventional wet spinning technique, and the gained fiber is done fracture strength 3.0～4.5cN/dtex, dried elongation at break 18～36%, 92～95 ℃ of water solution temperatures.And new technology gained finished fiber energy consumption has descended 32%, and manufacturing cost descends 800 yuan/ton.
Embodiment 2
With the degree of polymerization 1200 ± 50, the polyvinyl alcohol 40kg of alcoholysis degree 97mol% is after washing, add in the dissolution kettle with purifying waste water of 160kg, under agitation in 98 ± 2 ℃ of temperature, pressure-0.012Mpa, dissolve after 3 hours, after filtration, normal pressure deaeration 6～8 hours, make spinning solution in 98 ± 0.5 ℃ of temperature, after the measuring pump metering, be 0.08mm by the aperture, the spinning head ejection in 24000 holes, in bathing, 44 ± 1 ℃ saltcake are frozen into as-spun fibre, stretch 2.4 times through deflector roll, 1.5 times of damp and hot stretchings, tow is by demineralized water tank flush away saltcake, after preliminary treatment, enter in 220～250 ℃ the baking oven dry, pass through preheating then, 220～280 ℃ of xeothermic stretchings and HEAT SETTING, dried 1.25 times of the multiples that draw oil through machinery again, machine crimp, obtain fiber and do fracture strength 6.3cN/dtex, single fiber line density 1.5dtex, dried elongation at break 12～18%, 78～84 ℃ of water solution temperatures.
The comparative example 2, are raw material with the same size polyvinyl alcohol, adopt the conventional wet spinning technique, and the gained fiber is done fracture strength 3.0～4.5cN/dtex, dried elongation at break 20～36%, 87～90 ℃ of water solution temperatures.And new technology gained finished fiber energy consumption has descended 35%, and manufacturing cost descends 900 yuan/ton.
Embodiment 3
With the degree of polymerization 800 ± 50, the polyvinyl alcohol 35kg of alcoholysis degree 88mol% is after washing, add in the dissolution kettle with purifying waste water of 165kg, under agitation in 98 ± 2 ℃ of temperature, pressure-0.014Mpa, dissolve after 3 hours, after filtration, normal pressure deaeration 6～8 hours, make spinning solution 98 ± 0.5 ℃ of temperature, after the measuring pump metering, be 0.08mm by the aperture, the spinning head ejection in 30000 holes, in bathing, 44 ± 1 ℃ saltcake are frozen into as-spun fibre, stretch 2.4 times through deflector roll, 1.5 times of damp and hot stretchings, tow is by demineralized water tank flush away saltcake, after preliminary treatment, enter in 220～250 ℃ the baking oven dry, pass through preheating then, 220～280 ℃ of xeothermic stretchings and HEAT SETTING, dried 1.2 times of the multiples that draw oil through machinery again, machine crimp, obtain fiber and do fracture strength 5.8cN/dtex, line density 1.6dtex, dried elongation at break 13～20%, 70～74 ℃ of water solution temperatures.
The comparative example 3, are raw material with the same size polyvinyl alcohol, adopt the conventional wet spinning technique, and the gained fiber is done fracture strength 3.0～4.5cN/dtex, dried elongation at break 22～36%, 83～86 ℃ of water solution temperatures.And new technology gained finished fiber energy consumption has descended 38%, and manufacturing cost descends 980 yuan/ton.
Claims (4)
1. water-soluble polyvinyl alcohol fibers, it is by comprising following technical process preparation: the preparation of spinning solution, wet spinning, heat treatment process and spinning post processing is characterized in that
Heat treatment process is:
(1) washing: adopt the adverse current WATER-WASHING METHOD, fiber and soft water counter current contacting in rinsing bowl, washing temperature are controlled at 20～40 ℃, and fiber is saltcake adhesive rate≤1% after washing;
(2) preliminary treatment: adopt high-temperature resistant water dissolubility finish that fiber is carried out preliminary treatment, make fiber reach the technological requirement of heat treatment process;
(3) drying: 60～70% moisture content that contain on the fiber are removed;
(4) xeothermic stretching, typing: dried fiber is implemented xeothermic stretching after preheating, and carry out HEAT SETTING then and handle, 1～2 times of xeothermic stretching, heat setting temperature is 220～280 ℃, heat-setting time 1～5 minute;
The spinning last handling process is:
(1) oil: fiber oils by oiling machine;
(2) curl: adopt machine crimp technology, fiber oils after smooth preliminary treatment is carried out machine crimp by the machine crimp machine.
2. water-soluble polyvinyl alcohol fibers preparation technology comprises following process: the preparation of spinning solution, wet spinning, heat treatment process and spinning post processing, wherein
Heat treatment process is:
(1) washing: adopt the adverse current WATER-WASHING METHOD, fiber and soft water counter current contacting in rinsing bowl, washing temperature are controlled at 20～40 ℃, and fiber is saltcake adhesive rate≤1% after washing;
(2) preliminary treatment: adopt high-temperature resistant water dissolubility finish that fiber is carried out preliminary treatment, make fiber reach the technological requirement of heat treatment process;
(3) drying: 60～70% moisture content that contain on the fiber are removed;
(4) xeothermic stretching, typing: dried fiber is implemented xeothermic stretching after preheating, and carry out HEAT SETTING then and handle, 1～2 times of xeothermic stretching, heat setting temperature is 220～280 ℃, heat-setting time 1～5 minute;
The spinning last handling process is:
(1) oil: fiber oils by oiling machine;
(2) curl: adopt machine crimp technology; Fiber oils after smooth preliminary treatment is carried out machine crimp by the machine crimp machine.
3. water-soluble polyvinyl alcohol fibers, it is characterized in that with the degree of polymerization 800～2400, when the polyvinyl alcohol of alcoholysis degree 88～99mol% is the feedstock production water-soluble polyvinyl alcohol fibers, its fiber is done fracture strength 〉=5cN/dtex, dried elongation at break 10～20%, 60～90 ℃ of water solution temperatures, filament fiber number 1.0～8dtex, 8～12/25mm of crispation number.
4. the purposes of the described water-soluble polyvinyl alcohol fibers of claim 1, it is characterized in that this fiber is used for the production endless tow or is processed into wool top, with wool, sliver, fiber crops or chemical fibre blending, make high grade yarn or hollow yarn, or cut into staple fibre and do nonwoven fabric, penelope or papermaking.
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