CN1081686C - Wet PVA-crosslinking spinning technology - Google Patents
Wet PVA-crosslinking spinning technology Download PDFInfo
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- CN1081686C CN1081686C CN 98101364 CN98101364A CN1081686C CN 1081686 C CN1081686 C CN 1081686C CN 98101364 CN98101364 CN 98101364 CN 98101364 A CN98101364 A CN 98101364A CN 1081686 C CN1081686 C CN 1081686C
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- bath
- coagulating bath
- grams per
- polyvinyl alcohol
- per liters
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- Expired - Fee Related
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- 238000009987 spinning Methods 0.000 title claims abstract description 21
- 238000004132 cross linking Methods 0.000 title claims abstract description 8
- 238000005516 engineering process Methods 0.000 title claims description 12
- 239000000835 fiber Substances 0.000 claims abstract description 30
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 19
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 15
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 14
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 14
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 230000001112 coagulating effect Effects 0.000 claims description 19
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 150000003608 titanium Chemical class 0.000 claims description 3
- 150000003755 zirconium compounds Chemical class 0.000 claims description 3
- 230000015271 coagulation Effects 0.000 abstract description 4
- 238000005345 coagulation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052796 boron Inorganic materials 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- 229910052726 zirconium Inorganic materials 0.000 abstract description 2
- 229920002978 Vinylon Polymers 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 7
- 239000004568 cement Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000008961 swelling Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000004746 geotextile Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000003578 releasing effect Effects 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
本发明为聚乙烯醇湿法交联纺丝工艺，它以普通分子量聚乙烯醇为原料，以锆、硼、钛、硅组成复合交联剂，加水溶解后，在第一凝固浴中纺丝，在第二凝固浴中脱水、凝固。然后进行湿热牵伸，在酸浴中进行解交联处理，在中和浴中去除纤维中的酸和硫酸钠，经干燥，最后进行干热牵伸，总牵伸倍数达到15～18倍。制得的纤维强度为15克/旦，模量为360克/旦。本发明可使用现有维纶纺丝装置，工艺简单，便于推广，市场广阔。
The present invention is a polyvinyl alcohol wet cross-linking spinning process, which uses ordinary molecular weight polyvinyl alcohol as raw material, and uses zirconium, boron, titanium and silicon to form a composite cross-linking agent, which is dissolved in water and then spun in the first coagulation bath , dehydrated and coagulated in the second coagulation bath. Then carry out wet heat drawing, carry out decrosslinking treatment in an acid bath, remove acid and sodium sulfate in the fiber in a neutralization bath, dry, and finally carry out dry heat drawing, and the total drawing ratio reaches 15 to 18 times. The resulting fiber had a tenacity of 15 g/denier and a modulus of 360 g/denier. The present invention can use the existing vinylon spinning device, has simple process, is easy to popularize, and has a broad market.
Description
The present invention relates to a kind of method of producing the high-strength and high-modulus synthetic fiber, specifically, is to cooperate crosslinking agent to spin a kind of spinning technique method of high strength high modulus polyvinyl alcohol fiber by polyvinyl alcohol.
The polyvinyl alcohol raw material sources are extensive, have purposes widely, but improve its intensity and modulus, are still one of target that the synthetic fiber worker seek assiduously.For example vinal and cement have good cohesiveness and curable, can replace asbestos to be used to produce cement and strengthen goods, and it requires vinal to have higher intensity and modulus.At present, majority utilizes the vinal of wet spinning spinning high-strength and high-modulus both at home and abroad, generally the common molecular weight polyvinyl alcohol with DP=1750 ± 50 is a raw material, all use boron to make crosslinking agent, open with Chinese patent: CN1031727A " process for manufacturing of polyvinyl alcohol filaments " is an example, it discloses a kind of concentration 14～20% times, adds by weight 0.8～5.5% boric acid and 0.05～1.5% oxirane high polymer in polyvinyl alcohol, makes spinning solution.The order of its technical process is, earlier through coagulating bath, neutralization baths, damp and hot drawing-off, washing and drying then, and the dry heat drafting processing, thus the baked tensile strength that obtained for 6～300,000 dawn was 11.6 gram/dawn, 264 gram/dawn of initial modulus, the high-intensity fiber of degree of stretching 7.7%.But think that through practice its intensity, particularly modulus also have the possibility that improves.In addition, in order to improve the drawing-off performance, fiber mesoboric acid content is no more than 0.3% at most, and this has just increased the time that boric acid is removed in washing, causes fiber swelling and doubling, occurs lousiness and broken end when making dry heat drafting easily, influences the quality of continued operation and product.Similar therewith manufacture method, as the clear 47-42058 of Japan Patent, clear 54-32858, clear 59-43112 etc. all have this shortcoming.
The objective of the invention is to avoid the weak point of above-mentioned existence, provide a kind of employing polyvinyl alcohol common spinning technique, good spinnability, the washing time is short, the Wet PVA-crosslinking spinning technology that fibre strength and modulus are higher.
Purpose of the present invention can realize with the following method, its Wet PVA-crosslinking spinning technology at first is mixed with spinning solution with polyvinyl alcohol and crosslinking agent, its stoste consists of: polyvinyl alcohol concentration is 12～16%, crosslinking agent adds concentration 0.5～5%, used crosslinking agent is made up of in water miscible zirconium compounds, titanium salt, borate, the silicate two or more, the part by weight that adds is 3～5: 2～3.5: 1～2.5: 1～2.5 in turn, 95～98 ℃ of spinning temperatures; Solution sprays into coagulating bath through spinneret orifice and becomes silk, and its coagulating bath is made of first coagulating bath and second coagulating bath, and first coagulation bath composition is: NaOH: 15～50 grams per liters, sodium sulphate: 300～380 grams per liters, control temperature: 40～45 ℃; Second coagulation bath composition is: NaOH: 10～30 grams per liters, and sodium sulphate: 330～410 grams per liters, the control temperature is: 45～50 ℃, carry out 2～4 times of drawing-offs simultaneously; Order obtains the high-strength and high-modulus long filament through damp and hot drawing-off, acid bath, neutralization bath, drying, dry heat drafting then.
This law main purpose is to make fiber keep the uniformity of structure and good drawing-off performance when nascent state, the as-spun fibre outward appearance is similar to rounded cross section, adopt two coagulating baths: in first coagulating bath for this reason, it is certain crosslinked that big molecule is produced, avoided intermolecular random winding, making as-spun fibre keep gel state also slowly solidifies, reduce amount of sodium hydroxide in second coagulating bath, suitably increase sodium sulfate concentration, make the further dehydration, crosslinked of big molecular polyethylene alcohol, form the as-spun fibre of even structure, and carry out drawing-off first.For cooperating this technology, the selection of its crosslinking agent should make polyvinyl alcohol molecule crosslinked easily, and will satisfy the requirement of spinning technique to fiber.Crosslinking agent is used water miscible zirconium compounds, titanium salt, borate and silicate.In addition, owing to adopt two coagulating baths to form the uniform as-spun fibre of structure, good drawing-off performance is arranged among the present invention.
Purpose of the present invention can also realize that fiber enters damp and hot drawing-off bath after drawing-off first, keeps sodium sulfate concentration in the bath with following method: 340～380 grams per liters, and under 80～95 ℃ of temperature, 2～4 times of drawing-offs.Then enter acid bath, keep sodium sulfate concentration in the acid bath: 280～320 grams per liters, sulfuric acid concentration: 10～40 grams per liters, under effect of sulfuric acid, make the big molecule of polyvinyl alcohol produce crosslinked generating unit and decompose crosslinkedly, purpose is to improve the dry heat drafting performance of fiber.The fiber retention time is in neutralization is bathed: 20～90 seconds, purpose is flush away sulfuric acid and sodium sulphate, make fiber be neutral, this process time of staying comparison is shorter than the patented technology washing time, avoid fiber generation swelling, the high drafting that has guaranteed fiber has promptly guaranteed the high powerful feature that high drafting had, though still have certain corsslinking molecular, does not influence the drawing-off performance and can increase the intensity of product.Drying case control temperature is carried out drying for 120～150 ℃ again, and be drying time: 1～5 minute.At last, carry out dry heat drafting under 225～245 ℃, total drafting multiple can reach 15～18 times.Its drying and drawing-off can be adopted prior art, and its equipment therefor adopts the used device of prior art to transform a little and gets final product.
The present invention has the following advantages compared to existing technology: 1, with the homemade common polythene alcohol in DP1750 ± 50 is raw material, adopt zirconium, titanium, boron, silicon type multiple crosslinking agent and two coagulating bath wet method crosslinking spinning technology, can reach 15 gram/dawn high strength, the vinal of 360 gram/dawn high-moduluss, comparison improves 30% and 36% respectively than patented technology; The drawing-off performance is good, can reach 15～18 times, and comparison is than high about 2～5 times of patent.2, remaining crosslinking agent in the flush away fiber painstakingly not in neutralization is bathed not only can be avoided fiber generation swelling, and can keep insignificant, thereby improves the modulus of fiber.3, can be used for processing high-intensity product, as rope, shelter cloth, rotary hose, industrial sewing line, geotextiles, safety belt, lifting bag, conveyer belt, material for core, fire-retardant product etc., can also be as asbestos alternative, be used to produce cement and other refinforced cement composites, have market widely at home and abroad.
The drawing of accompanying drawing of the present invention is described as follows:
Accompanying drawing is a process flow diagram of the present invention.
Following conjunction with figs. illustrates the present invention with embodiment, and for easier popularization, we use the most frequently used degree of polymerization DP 1750 ± 50, and alcoholysis degree 99.9% polyvinyl alcohol is made the aqueous solution of concentration 14%.2% multiple crosslinking agent of polyvinyl alcohol weight is added in the solution, and multiple crosslinking agent is selected zirconium sulfate, sodium tetraborate for use, and it consists of zirconium sulfate: sodium tetraborate=3: 2.Polyvinyl alcohol spin dope is that 0.08 millimeter spinneret orifice 1 is clamp-oned contains sodium sulfate 370 grams per liters, NaOH 30 grams per liters by the aperture, temperature is 45 ℃ first coagulating bath 2, form the gel as-spun fibre, its process flow diagram is seen accompanying drawing, then enter sodium sulphate 400 grams per liters, NaOH 15 grams per liters, second coagulating bath 3 that temperature is 45 ℃, further dewater, solidify, and 2.5 times of drawing-offs.Sodium sulphate 360 grams per liters in 4,90 ℃ of temperature, 2 times of drawing-offs are bathed in damp and hot drawing-off.Enter contains sodium sulfate 280 grams per liters then, the acid bath 5 of sulfuric acid 15 grams per liters, 1.4 times of room temperature drawing-offs make crosslinked releasings a large amount of in the fiber in drawing-off.The neutralization that enters room temperature then bathes 6, and sodium sulphate in the flush away fiber and sulfuric acid stopped 30 seconds in neutralization is bathed.Then dry in 140 ℃ of drying boxes 7, enter 235 ℃ of dry heat drafting casees 8 afterwards and carry out dry heat drafting, make fiber total draft multiple reach 16 times.Make fiber after measured, intensity was 15 gram/dawn, and at the 360 gram/dawn of modulus, extension at break is 6.0%, and fiber number is 1.48 dtexs.Whole technology continued operation since with the spinning technique basically identical of existing homemade polyvinyl, can utilize former polyvinyl process units, change a little and can produce high strength high modulus polyvinyl alcohol fiber.
Annotate: indication of the present invention " % " is all percentage by weight.
Claims (2)
1, a kind of Wet PVA-crosslinking spinning technology, be mixed with spinning solution by polyvinyl alcohol and crosslinking agent, through spinneret orifice (1) Cheng Sihou, enter coagulating bath (2), (3) and drawing-off, bathe (4), acid bath (5), neutralization bath (6), dry (7) through damp and hot drawing-off then, dry heat drafting (8) technical process obtains the high-strength and high-modulus long filament, it is characterized in that: 1. the spinning solution percentage by weight consists of: polyvinyl alcohol concentration is 12-16%, crosslinking agent adds concentration 0.5～5%, 95～98 ℃ of spinning temperatures; 2. its anterior technical process is: spinning solution is behind spinneret orifice (1), and order is bathed (4), acid bath (5), neutralization bath (6) through first, second coagulating bath (2), (3), damp and hot drawing-off; 3. its coagulating bath is made up of first coagulating bath (2) and second coagulating bath (3), and first coagulating bath (2) contains: NaOH: 15～50 grams per liters, sodium sulphate: 300～380 grams per liters, control temperature: 40～45 ℃; Second coagulating bath (3) contains: NaOH: 10～30 grams per liters, and sodium sulphate: 330～410 grams per liters, the control temperature is: 45～50 ℃, the 2-4 of drawing-off simultaneously is doubly; 4. used crosslinking agent is made up of in water miscible zirconium compounds, titanium salt, borate, the silicate two or more, and the part by weight of adding is in turn: 3～5: 2～3.5: 1～2.5: 1～2.5.
2, Wet PVA-crosslinking spinning technology according to claim 1 is characterized in that fiber with the time is: 20～90 seconds in neutralization bath (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98101364 CN1081686C (en) | 1998-04-14 | 1998-04-14 | Wet PVA-crosslinking spinning technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98101364 CN1081686C (en) | 1998-04-14 | 1998-04-14 | Wet PVA-crosslinking spinning technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1197858A CN1197858A (en) | 1998-11-04 |
| CN1081686C true CN1081686C (en) | 2002-03-27 |
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ID=5216646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98101364 Expired - Fee Related CN1081686C (en) | 1998-04-14 | 1998-04-14 | Wet PVA-crosslinking spinning technology |
Country Status (1)
| Country | Link |
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| CN (1) | CN1081686C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422404C (en) * | 2006-07-27 | 2008-10-01 | 中国石化集团资产经营管理有限公司重庆天然气化工分公司 | A kind of wear-resistant polyvinyl acetal fiber and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6743273B2 (en) | 2000-09-05 | 2004-06-01 | Donaldson Company, Inc. | Polymer, polymer microfiber, polymer nanofiber and applications including filter structures |
| CN101117736A (en) * | 2000-09-05 | 2008-02-06 | 唐纳森公司 | Polymer, polymer microfiber, polymer nanofiber and use including filter structure |
| FR2828500B1 (en) * | 2001-08-08 | 2004-08-27 | Centre Nat Rech Scient | PROCESS FOR REFORMING COMPOSITE FIBERS AND APPLICATIONS |
| CN100390333C (en) * | 2006-01-17 | 2008-05-28 | 中国石化集团资产经营管理有限公司重庆天然气化工分公司 | Method and device for manufacturing vinylon filament bundle |
| CN103060940B (en) * | 2011-10-18 | 2015-09-30 | 中国石油化工集团公司 | A kind of preparation method of medium modulus vinal |
| CN103276469B (en) * | 2013-05-23 | 2015-02-25 | 永安市宝华林实业发展有限公司 | Production method of concrete reinforced and toughened PVA (polyvinyl alcohol) fiber |
| CN106757403A (en) * | 2015-11-19 | 2017-05-31 | 张家港市宏盛贸易有限公司 | Spinning equipment before water-soluble fibre |
| CN111101219B (en) * | 2018-10-26 | 2022-08-12 | 中国石油化工股份有限公司 | High-strength high-modulus polyvinyl alcohol filament and preparation method thereof |
| CN111636114B (en) * | 2020-06-12 | 2021-08-31 | 东华大学 | Preparation of a high-strength and high-conductivity polyvinyl alcohol/graphene composite fiber |
| CN112095170B (en) * | 2020-08-04 | 2022-03-25 | 东华大学 | LaCl3Cross-linked high-strength high-modulus polyvinyl alcohol fiber and preparation method thereof |
| CN112226840B (en) * | 2020-08-04 | 2021-07-23 | 东华大学 | A kind of high-strength and high-modulus PVA fiber and preparation method thereof |
-
1998
- 1998-04-14 CN CN 98101364 patent/CN1081686C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422404C (en) * | 2006-07-27 | 2008-10-01 | 中国石化集团资产经营管理有限公司重庆天然气化工分公司 | A kind of wear-resistant polyvinyl acetal fiber and its preparation method and application |
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| Publication number | Publication date |
|---|---|
| CN1197858A (en) | 1998-11-04 |
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