CN101812744A - Formalizing method of high-strength and high-modulus polyvinyl alcohol fiber - Google Patents
Formalizing method of high-strength and high-modulus polyvinyl alcohol fiber Download PDFInfo
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- CN101812744A CN101812744A CN200910065703A CN200910065703A CN101812744A CN 101812744 A CN101812744 A CN 101812744A CN 200910065703 A CN200910065703 A CN 200910065703A CN 200910065703 A CN200910065703 A CN 200910065703A CN 101812744 A CN101812744 A CN 101812744A
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Abstract
The invention discloses a formalizing method of high-strength and high-modulus polyvinyl alcohol fiber, which comprises the following steps: (1) preparing a swelling medium: dissolving 1-50 parts by weight of additive in 100 parts by weight of water and stirring to obtain the swelling medium; (2) pre-swelling the fiber: feeding the polyvinyl alcohol fiber bundle into the swelling medium to be swelled, wherein the temperature of the swelling medium is 20-80 DEG C and the swelling time is 10 to 60 minutes; and (3) formalizing the swelling fiber bundle: formalizing the swelled fiber bundle in an aldehyde condensation solution, wherein the formalizing temperature is 40-90 DEG C and the formalizing time is 10-40 min. The formalized polyvinyl alcohol fiber can be manufactured into short fiber or filament after being processed. The formalized high-strength and high-modulus polyvinyl alcohol fiber can be purely spun or blended with other fibers to manufacture textile threads and fabrics with various specifications, which are used for manufacturing high-strength wear-resistant work clothes, training clothes, tents, backpacks, ropes and the like, and has good popularization and application prospects.
Description
Technical field
The present invention relates to a kind of formalizing method of high strength high modulus polyvinyl alcohol fiber, belong to the manufacturing technology field of high-performance fiber.
Background technology
Polyvinyl alcohol is a kind of function admirable, and broad-spectrum polymer was once greatly developed vinal in order to solve the people's clothing problem in Japan, Korea, China etc.But along with the emergence of the better terylene of serviceability, polyamide fibre and acrylic fibers with catch up from behind, vinal is owing to exist shortcomings such as wrinkle resistance is poor, size instability, dyeability difference, is subjected to bigger restriction in the application of garment industry.
Polyvinyl alcohol is because its special structure, has the potentiality of high-strength and high-modulusization with the fiber of its preparation, so various countries change in the developmental research of high strength high modulus polyvinyl alcohol fiber one after another, and obtained numerous achievements.Adopt the polyvinyl alcohol raw material of high molecular, high tacticity or adopt special spinning process to obtain the vinal of various high-strength and high-modulus.The manufacture method of all kinds of high-strength and high-modulus PAV fibers mainly contains following several: (1) wet method adds boron spinning (JP H10-046428 (1998), JP S37-14422 (1962)); (2) dry-wet spinning (JP H07-207521 (1995), JP H03-023004 (1991), JPH02-300308 (1990); (3) gel spinning (CN 87103211, CN 1092120A, JPS61-289112 (1986) A2); (4) crosslinking spinning (Zhu Bensong, polyvinyl communication, 1992,12 the 4th phases of volume).Above-mentioned several method has common characteristic: promptly be control or the entanglement of reduction fiber molecule interchain and the degree of crystallinity of fiber in spinning process, then in the post processing of fiber, carry out super drawing and make fiber obtain high-orientation and degree of crystallinity, thereby make fiber obtain excellent performance.Characteristics such as the intensity high-modulus is big because of having for the polyvinyl alcohol high-strength high-modulus fibre, low depth, anti-daylight, good weatherability, hydrophily are strong, make it purposes widely be arranged, can also do tire cord, belt, rotary hose, rope, reinforced plastics and rubber reinforcing material etc. simultaneously in building trade.
The high strength high modulus polyvinyl alcohol fiber fiber generally all has higher softening point in water temperature because degree of crystallinity is very high, and it is mainly used in industry, building field, therefore often it is not carried out formalizing and handles and directly use.But when reality was used, though this fibrid has high intensity and modulus, its elongation at break was very low, and hot water resistance is not good yet, so this fibrid and be not suitable for being applied to clothes and use under some hot and humid environments.In order to expand its Application Areas, be necessary to develop suitable formalizing technology and promote its hot water resistance and degree of stretching.Because high strength high modulus polyvinyl alcohol fiber compact structure, the degree of crystallinity height, degree of orientation height, micromolecule is difficult to be penetrated into fibrous inside, adopt conventional formalizing method that the hydroxyl in the fiber unformed area is effectively sealed, the fiber degree of formalization is lower, the still not anti-boiling water of the fiber after the hydroformylation.
Summary of the invention
The object of the present invention is to provide a kind of formalizing method of high strength high modulus polyvinyl alcohol fiber, so that obtain more greatly degree of stretching and hot water resistance high strength high modulus polyvinyl alcohol fiber preferably.
To achieve these goals, technical scheme of the present invention has adopted a kind of formalizing method of high strength high modulus polyvinyl alcohol fiber, may further comprise the steps:
(1) swelling medium preparation
With weight portion is that the additive of 1-50 part is dissolved in 100 parts the water, stirs and makes the swelling medium;
(2) the pre-swelling treatment of fiber
The vinal tow is sent into the swelling medium carry out swelling, 20-80 ℃ of swelling medium temperature, 10～60 minutes swelling treatment time;
(3) formalizing of swelling tow is handled
Carry out formalizing through the fibre bundle after the swelling in hydroformylation liquid and handle, wherein the hydroformylation temperature is 40-90 ℃, hydroformylation time 10-40min.
Described additive is an acid solution.
Described additive is any or the arbitrarily combination in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid and the formic acid.
Described hydroformylation liquid is prepared from by the component of following parts by weight: 20～80 parts in formaldehyde, 100～300 parts in sulfuric acid, 100～400 parts in sodium sulphate.
Described vinal is by adding boron spinning, dry-wet spinning, gel spinning or the preparation of crosslinking spinning method.
The fibre number of described vinal is 1-10dtex, intensity 10-25cN/dtex, and modulus is 120-600cN/dtex, elongation at break≤12%, the softening point in water temperature is 95-105 ℃.
Implement formalizing after adopting method of the present invention that high strength high modulus polyvinyl alcohol fiber through adding methods acquisitions such as boron spinning, dry-wet spinning, gel spinning, crosslinking spinning is carried out pre-swelling treatment, high strength high modulus polyvinyl alcohol fiber through pre-swelling treatment is easy to carry out the formalizing processing, can use comparatively soft condition that fiber is carried out formalizing, saved production cost greatly, reduced equipment corrosion has been shortened the production cycle; Fiber behind formalizing has kept the characteristic of most of high-strength and high-modulus, and degree of stretching is bigger, and hot water resistance also significantly increases, and makes fiber have more wide Application Areas; Pre-swelling treatment process is easy, and technological process is short.Vinal of the present invention can be processed into staple fibre or long filament after handling through formalizing after treatment.Fibre number is 1-10dtex, intensity 8-18cN/dtex, and modulus is 100-400cN/dtex, elongation at break 10%-25%, the softening point in water temperature is 110-125 ℃, boiling water shrinkage≤5%.High strength high modulus polyvinyl alcohol fiber after the employing formalizing is handled can purely spin or make spinning of all size and lining with other fiber blends, be used to make high-strength wearable Work Clothes, BDU, tent, knapsack and rope etc., have good popularization and application prospect.
The specific embodiment
Embodiment 1
PVA1799 is added the boron spinning through wet method, making fibre number is 1.5dtex, fracture strength 11.5cN/dtex, elongation at break 8%, modulus is 140cN/dtex, and the RP value is 97 ℃ a high strength high modulus polyvinyl alcohol fiber, gets 30kg concentration and is 98% the concentrated sulfuric acid and be dissolved in and make the swelling medium in the 1000kg water, aforementioned high-strength high-modulus fibre soaked place the swelling medium, pre-swelling treatment is 30 minutes under 40 ℃, and then pre-swelling silk carries out formalizing by continuous nervous acetalizing machine to be handled, and the hydroformylation formula of liquid is: formaldehyde 40g/l, sulfuric acid 240g/l, sodium sulphate 210g/l, 65 ℃ of hydroformylation temperature, hydroformylation time 20min, fiber after the hydroformylation is through neutralization, washing oils, and can be made into staple fibre or long filament after the drying, the fiber index is as follows: fibre number 1.6dtex, intensity 9.5cN/dtex, initial modulus are 120cN/dtex, elongation at break 20%, softening temperature is 112 ℃ in the water, boiling water shrinkage 3%.
Embodiment 2
PVA2099 is added the boron spinning through wet method, making fibre number is 1.7dtex, fracture strength 13cN/dtex, elongation at break 7%, modulus is 150cN/dtex, the RP value is 97 ℃ a high strength high modulus polyvinyl alcohol fiber, gets 10kg concentration and is 37% hydrochloric acid and be dissolved in and make pre-swelling medium in the 1000kg water, aforementioned high-strength high-modulus fibre is soaked place the swelling medium 30 ℃ of pre-swelling treatment 40 minutes down, then pre-swelling silk carries out formalizing by continuous nervous acetalizing machine to be handled, the hydroformylation formula of liquid is: formaldehyde 45g/l, sulfuric acid 250g/l, sodium sulphate 200g/l, 70 ℃ of hydroformylation temperature, hydroformylation time 25min, the fiber after the hydroformylation wash through neutralization, oil, can be made into staple fibre or long filament after the drying, the fiber index is as follows: fibre number 1.75dtex, intensity 10.5cN/dtex, initial modulus is 125cN/dtex, elongation at break 16%, softening temperature is 115 ℃ in the water, boiling water shrinkage 3%.
Embodiment 3
With PVA6099 through dry-wet spinning,-20 ℃ of methyl alcohol are done coagulating bath, making fibre number is 2.5dtex, fracture strength 18cN/dtex, elongation at break 7%, modulus are 330cN/dtex, and the RP value is 102 ℃ a high strength high modulus polyvinyl alcohol fiber, getting 100kg concentration and be 98% the concentrated sulfuric acid is dissolved in and makes pre-swelling solution in the 1000kg water, aforementioned high-strength high-modulus fibre soaked place swelling 60 ℃ of following pre-swelling treatment 30 minutes, then pre-swelling silk carries out formalizing by continuous nervous acetalizing machine to be handled, and the hydroformylation formula of liquid is: formaldehyde 40g/l, sulfuric acid 260g/l, sodium sulphate 180g/l, 70 ℃ of hydroformylation temperature, hydroformylation time 25min, fiber after the hydroformylation is through neutralization, washing oils, and can be made into staple fibre or long filament after the drying, the fiber index is as follows: fibre number 2.6dtex, intensity 12.5cN/dtex, initial modulus are 240cN/dtex, elongation at break 14%, softening temperature is 118 ℃ in the water, boiling water shrinkage 2%.
It should be noted last that: above embodiment is only in order to explanation, and unrestricted technical scheme of the present invention, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (6)
1. the formalizing method of a high strength high modulus polyvinyl alcohol fiber is characterized in that: may further comprise the steps:
(1) swelling medium preparation
With weight portion is that the additive of 1-50 part is dissolved in 100 parts the water, stirs and makes the swelling medium;
(2) the pre-swelling treatment of fiber
The vinal tow is sent into the swelling medium carry out swelling, 20-80 ℃ of swelling medium temperature, 10～60 minutes swelling treatment time;
(3) formalizing of swelling tow is handled
Carry out formalizing through the fibre bundle after the swelling in hydroformylation liquid and handle, wherein the hydroformylation temperature is 40-90 ℃, hydroformylation time 10-40min.
2. the formalizing method of high strength high modulus polyvinyl alcohol fiber according to claim 1, it is characterized in that: described additive is an acid solution.
3. the formalizing method of high strength high modulus polyvinyl alcohol fiber according to claim 2 is characterized in that: described additive is any or the combination arbitrarily in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid and the formic acid.
4. the formalizing method of high strength high modulus polyvinyl alcohol fiber according to claim 1, it is characterized in that: described hydroformylation liquid is prepared from by the component of following parts by weight: 20～80 parts in formaldehyde, 100～300 parts in sulfuric acid, 100～400 parts in sodium sulphate.
5. the formalizing method of high strength high modulus polyvinyl alcohol fiber according to claim 1 is characterized in that: described vinal is by adding boron spinning, dry-wet spinning, gel spinning or the preparation of crosslinking spinning method.
6. according to the formalizing method of arbitrary described high strength high modulus polyvinyl alcohol fiber among the claim 1-5, it is characterized in that: the fibre number of described vinal is 1-10dtex, intensity 10-25cN/dtex, modulus is 120-600cN/dtex, elongation at break≤12%, softening point in water temperature are 95-105 ℃.
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| CN200910065703A CN101812744A (en) | 2009-08-10 | 2009-08-10 | Formalizing method of high-strength and high-modulus polyvinyl alcohol fiber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774266A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工集团公司 | Preparation method of polyvinyl formal fiber |
| CN107287668A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of heat-resistance type PVA fibers and application thereof |
| CN107287669A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of alkaline-resisting temperature resistance PVA fibers and application thereof |
-
2009
- 2009-08-10 CN CN200910065703A patent/CN101812744A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774266A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工集团公司 | Preparation method of polyvinyl formal fiber |
| CN107287668A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of heat-resistance type PVA fibers and application thereof |
| CN107287669A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of alkaline-resisting temperature resistance PVA fibers and application thereof |
| CN107287668B (en) * | 2016-04-12 | 2019-08-30 | 中国石油化工集团公司 | A kind of heat-resistance type PVA fiber and application thereof |
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Application publication date: 20100825 |