CN100427653C - Prepn and application of jelly fiber of polyethylene in ultrahigh molecular weight - Google Patents
Prepn and application of jelly fiber of polyethylene in ultrahigh molecular weight Download PDFInfo
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- CN100427653C CN100427653C CNB2006101187330A CN200610118733A CN100427653C CN 100427653 C CN100427653 C CN 100427653C CN B2006101187330 A CNB2006101187330 A CN B2006101187330A CN 200610118733 A CN200610118733 A CN 200610118733A CN 100427653 C CN100427653 C CN 100427653C
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Abstract
The present invention relates to preparation process and application of jelly fiber of polyethylene in ultrahigh molecular weight. The preparation process includes the following steps: pre-treatment of jelly fiber with hydrocarbon extractant; continuous extraction; pumping the solvent/ extractant mixture with one conveying pump from the bath and the ultrasonic extracting tank to the fractioning recovery unit and recovering; returning the recovered extractant to the bath and the ultrasonic extracting tank; and filtering and depurating the solvent and returning the solvent to the dissolving step. The high strength and high modulus polyethylene fiber is used widely in pulletproof vest, rope, parachute, sports equipment and fishing line.
Description
Technical field
The invention belongs to the high-performance fiber technical field, the preparation method and the application of particularly a kind of ultra-high molecular weight polyethylene (PE) gel fiber.
Background technology
The spinning of existing employing super high molecular weight polyethylene gel prepares in the technology of high-performance fiber, the recovery of solvent is to adopt extracting process in fibre forming process and the gel fiber, promptly non-volatile first solvent exchange is come out with volatilizable second auxiliary agent, what the method for eliminating volatility second auxiliary agent was implemented in one dry heat processing in back and drawing process afterwards.When solvent generally adopted higher boiling mineral oil (white oil) or paraffin oil, kerosene etc., the second auxiliary agent extractant then adopted low boilers, as dimethylbenzene, gasoline, chloroform, tetrachloro-ethylene, acetone, trichorotrifluoroethane etc.Its defective is except extraction cost height, and cost recovery is big, and equipment investment is big, and is inflammable and explosive outer or because of environmental protection or because of safety problem, and capital fund and environmental protection are brought harsh requirement.
Summary of the invention
The purpose of this invention is to provide the preparation method and the application of a kind of ultra-high molecular weight polyethylene (PE) gel fiber, comprise extractant, extracting process and recovery method,, improve output, stable fibers quality and safety in production to overcome the defective of prior art.
The preparation method of a kind of ultra-high molecular weight polyethylene gel fiber of the present invention comprises the steps:
(1) gel fiber carries out preliminary treatment in the bath device of static, spray that the hydrocarbon extractant is housed or tape drum bubble, tow advances speed a 0.5～3m/min, the gel fiber pretension is greater than 0.02g/d, room temperature to 50 ℃, the extractant flash-point is below 300 ℃, and boiling point is at the hydrocarbon more than 7 ℃;
(2) in pretreated gel fiber is being equipped with the multiple tracks extraction tank of hydrocarbon extractant, extract again continuously, be furnished with Vltrasonic device in the extraction tank, advance speed a 0.8～8m/min, 50～70 ℃ of temperature.After the multiple tracks extraction, the frozen glue tow of extraction contains quantity of solvent has reduced to below 5%, and solvent and extractant direct and back road drying, stretching device produce after simple filtration trace solvent, extractant are delivered to retracting device together.Fibre bundle through extraction is directly delivered to down road drying, stretching process;
(3) be quantitatively transferred to the fractionation retracting device by the solvent/extractant mixture that produces in bath and the ultrasonic extraction groove by delivery pump, the extractant that fractionation is reclaimed can directly be delivered to respectively in extraction bath and the ultrasonic extraction groove with pump, and solvent after filtration, take off and deliver to preceding road dissolution process after assorted.
Technological process of the present invention is: PE gel fiber → boundling tension bracket → minute guide frame → pressing oil roll → hydrocarbon liquid preliminary treatment bath (mode such as static, spray or bubbling) → hydrocarbon extraction tank → heated-air drying of seven roller carry-over pinch rolls → ultrasonic waves → multistage stretching → postprocessing working procedures such as coiling.
Ultrasonic intensity 5-50w/m in the described step (2)
2, advance speed 0.8～8m/ branch, 50～70 ℃ of temperature, total draw ratio 10-100 is doubly.
One draft temperature: 105～135 ℃; 1～5 times of multiplying power
Two road draft temperatures: 115～155 ℃; 2～5 times of multiplying powers
Three road draft temperatures: 125～155 ℃; 1.5～4 times of multiplying powers
Four road heat setting temperatures: 125～155 ℃.
The application of a kind of ultra-high molecular weight polyethylene gel fiber of the present invention (PE fiber):
Be used for bulletproof anti-puncturing dress material, rope, parachute, setline, athletic sports appliance framework material etc.Beneficial effect:
1, handle through preliminary treatment bath and supersonic oscillations extraction, the solvent that has guaranteed gel fiber is by fully effectively displacement, and the saving of the next procedure energy, and hydrocarbon is nonpoisonous and tasteless, has guaranteed safety of operators.
2, the online fractionation recovery system of the company's of employing machine, the solvent naphtha and the extractant hydrocarbon that constantly will extract in the gel fiber separate recovery, be delivered to after filtering in preliminary treatment bath and the supersonic oscillations continuous extraction with the extractant hydrocarbon after be about to reclaiming and recycle, and solvent is directly delivered to preceding road dissolution process after filtering, thereby helps reducing production costs.
3, the high-strength and high-modulus PE fiber that adopts extractant of the present invention and method to produce, steady quality, cost is low, can be widely used in bulletproof anti-puncturing dress material, rope, parachute, setline, the athletic sports appliance framework material.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Raw material: by the ultra-high molecular weight polyethylene gel fiber that spinning workshop section makes, 240f, oil content is about 85%, and it is 18 strands that boundling divides number of share of stock; Pressing oil roll tension force: 0.5kg/cm
2, extractant adopts hydrocarbon EXXSOL D-40, preliminary treatment bath vapour pressure 0kg/cm
2, 30 ℃ of preliminary treatment bath temperature, drying enters stretching process after handling (baking temperature).One draw speed 3.5m/min, stretching ratio: 3.5 times, 105 ℃ of ultrasonic extraction bath temperatures, 5 minutes time, ultrasonic intensity 20w/m
2, two road draw speed 13m/min, 3.7 times of stretching ratios, 125 ℃ of draft temperatures.Three road draw speed 29m/min, stretching ratio: 2.23 times, 135 ℃ of draft temperatures.29 times of total draw ratios.145 ℃ of four road heat setting temperatures.Record the powerful 28cN/dtex of super high molecular weight high-strength high-modulus polyethylene fiber; Extension at break 5.2%, modulus 980cN/dtex, solvent 1.8%.
Embodiment 2
Raw material: by the ultra-high molecular weight polyethylene gel fiber that spinning workshop section makes, 240f, oil content is about 85%, and boundling divides number of share of stock: 18 strands; Pressing oil roll tension force 0.5kg/cm
2Extractant adopts hydrocarbon EXXSOL D-40, preliminary treatment bath air pressure 0.5kg/cm
230 ℃ of preliminary treatment bath temperature, drying enters stretching process after handling (baking temperature).One draw speed: 3.5m/min, stretching ratio: 3.5 times; 105 ℃ of ultrasonic extraction bath temperatures, 5 minutes time, ultrasonic intensity: 25w/m
2Two road draw speed 13m/min, stretching ratio 3.7; 125 ℃ of draft temperatures.Three road draw speed 29m/min, 2.23 times of stretching ratios, 135 ℃ of draft temperatures.29 times of total draw ratios.145 ℃ of four road heat setting temperatures.Record the powerful 29.7cN/dtex of super high molecular weight high-strength high-modulus polyethylene fiber; Extension at break 4.9%, modulus 1020cN/dtex, solvent 1.4%.
Embodiment 3
Raw material: by the ultra-high molecular weight polyethylene gel fiber that spinning workshop section makes, the 240f/ thigh, oil content is about 85%, and boundling divides 18 strands of number of share of stocks; Pressing oil roll tension force 0.5kg/cm
2Extractant adopts hydrocarbon EXXSOL D-40, preliminary treatment bath air pressure: 1.0kg/cm
2, 30 ℃ of preliminary treatment bath temperature; Drying enters stretching process after handling (baking temperature).One draw speed 3.5m/min; 3.5 times of stretching ratios; 105 ℃ of ultrasonic extraction bath temperatures, 5 minutes time, ultrasonic intensity 30w/m
2, two road draw speed 13m/min, 3.7 times of stretching ratios; 125 ℃ of draft temperatures.Three road draw speed 29m/min, 2.23 times of stretching ratios, 135 ℃ of draft temperatures, 29 times of total draw ratios.145 ℃ of four road heat setting temperatures.Record the powerful 31.2cN/dtex of super high molecular weight high-strength high-modulus polyethylene fiber; Extension at break 4.2%, modulus 1220cN/dtex, solvent 1.2%.
Comparative Examples 1
Raw material: by the ultra-high molecular weight polyethylene gel fiber that spinning workshop section makes, the 240f/ thigh, oil content is about 85%, and it is 18 strands that boundling divides number of share of stock.Except the hydrocarbon extractant is changed into 120 gasoline, extraction is identical with embodiment 3 with drawing process.Record the powerful 28cN/dtex of super high molecular weight high-strength high-modulus polyethylene fiber; Extension at break 5.8%, modulus 970cN/dtex, solvent 4.2%.
Comparative Examples 2
Raw material: by the ultra-high molecular weight polyethylene gel fiber that spinning workshop section makes, the 240f/ thigh, oil content is about 85%, and it is 18 strands that boundling divides number of share of stock.Except the hydrogen compound extractant is changed into the dimethylbenzene, extraction is identical with embodiment 3 with drawing process.Record the powerful 28.5cN/dtex of super high molecular weight high-strength high-modulus polyethylene fiber; Extension at break 5.5%, modulus 1020cN/dtex, solvent 3.8%.
Claims (4)
1. the preparation method of a ultra-high molecular weight polyethylene (PE) gel fiber comprises the steps:
(1) gel fiber carries out preliminary treatment in the bath device of static, spray that the hydrocarbon extractant is housed or tape drum bubble, and tow advances speed a 0.5～3m/min, and the gel fiber pretension is greater than 0.02g/d, room temperature to 50 ℃;
(2) in being equipped with the multiple tracks extraction tank of hydrocarbon extractant, pretreated gel fiber extracts again continuously, is furnished with Vltrasonic device in the extraction tank, advance speed a 0.8～8m/min, 50～70 ℃ of temperature, after the multiple tracks extraction, the frozen glue tow of extraction contains quantity of solvent and has reduced to below 5%, solvent and extractant direct and back road drying, stretching device produce after simple filtration trace solvent, extractant are delivered to retracting device together, directly deliver to down road drying, stretching process through the fibre bundle of extraction;
(3) be quantitatively transferred to the fractionation retracting device by the solvent/extractant mixture that produces in bath and the ultrasonic extraction groove by delivery pump, the extractant that fractionation is reclaimed can directly be delivered to respectively in extraction bath and the ultrasonic extraction groove with pump, and solvent after filtration, take off and deliver to preceding road dissolution process after assorted.
2. according to the preparation method of the described a kind of ultra-high molecular weight polyethylene of claim 1 (PE) gel fiber: it is characterized in that: described extractant flash-point is below 300 ℃, and boiling point is at the hydrocarbon more than 7 ℃.
3. according to the preparation method of claim 1 or 2 described a kind of ultra-high molecular weight polyethylene (PE) gel fibers: it is characterized in that: described hydrocarbon is EXXSOL D-40.
4. according to the preparation method of the described a kind of ultra-high molecular weight polyethylene of claim 1 (PE) gel fiber: it is characterized in that: the ultrasonic intensity 5-50w/m in the described step (2)
2, advance speed 0.8～8m/ branch, 50～70 ℃ of temperature, total draw ratio 10-100 times,
One draft temperature: 105～135 ℃; 1～5 times of multiplying power
Two road draft temperatures: 115～155 ℃; 2～5 times of multiplying powers
Three road draft temperatures: 125～155 ℃; 1.5～4 times of multiplying powers
Four road heat setting temperatures: 125～155 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101187330A CN100427653C (en) | 2006-11-24 | 2006-11-24 | Prepn and application of jelly fiber of polyethylene in ultrahigh molecular weight |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101187330A CN100427653C (en) | 2006-11-24 | 2006-11-24 | Prepn and application of jelly fiber of polyethylene in ultrahigh molecular weight |
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| CN1974891A CN1974891A (en) | 2007-06-06 |
| CN100427653C true CN100427653C (en) | 2008-10-22 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135069B (en) * | 2007-09-29 | 2011-04-27 | 江苏神泰科技发展有限公司 | High-modulus high-strength polyvinyl fibre abstraction drafting production line |
| CN101230499B (en) * | 2008-02-26 | 2010-10-06 | 山东爱地高分子材料有限公司 | Coloured high-strength polyethylene fibre and method for manufacturing same |
| CN103103834A (en) * | 2011-11-15 | 2013-05-15 | 李胜春 | Preparation method of special rope in field of sports |
| CN106065497B (en) * | 2016-07-25 | 2018-07-27 | 江阴市五洋化工有限公司 | 125~155 DEG C of fractions are as the application and its extracting method for preparing high-strength polyethylene fiber extractant in mixed solvent oil |
| CN110117820A (en) * | 2019-04-16 | 2019-08-13 | 山东莱威新材料有限公司 | A kind of preparation method of spray process extraction high-strength high-modulus polyethylene gel spun fiber |
| CN113529212B (en) * | 2021-06-28 | 2023-05-02 | 上海化工研究院有限公司 | Method and device for rapidly separating solvent from ultra-high molecular weight polyethylene fiber |
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| CN1056544A (en) * | 1990-05-14 | 1991-11-27 | 中国纺织大学 | The preparation method of high-strength, high-modulus polyethylene fiber |
| CN1448546A (en) * | 2002-04-01 | 2003-10-15 | 阎镇达 | Method for spinning ultra -high strength ultra-high modules polyethylene fibre |
| CN1693545A (en) * | 2005-06-03 | 2005-11-09 | 北京特斯顿新材料技术发展有限公司 | Supercritical extraction and drying method in preparation of ultrahigh molecular weight polyethylene fibre |
| CN1246511C (en) * | 2002-12-27 | 2006-03-22 | 东华大学 | Extracting and drying process for superhigh relative molecular weight polyvinyl gel fibre |
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2006
- 2006-11-24 CN CNB2006101187330A patent/CN100427653C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056544A (en) * | 1990-05-14 | 1991-11-27 | 中国纺织大学 | The preparation method of high-strength, high-modulus polyethylene fiber |
| CN1448546A (en) * | 2002-04-01 | 2003-10-15 | 阎镇达 | Method for spinning ultra -high strength ultra-high modules polyethylene fibre |
| CN1246511C (en) * | 2002-12-27 | 2006-03-22 | 东华大学 | Extracting and drying process for superhigh relative molecular weight polyvinyl gel fibre |
| CN1693545A (en) * | 2005-06-03 | 2005-11-09 | 北京特斯顿新材料技术发展有限公司 | Supercritical extraction and drying method in preparation of ultrahigh molecular weight polyethylene fibre |
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| Title |
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| 超高分子量聚乙烯冻胶纤维的制备. 尹德荟，李炳海等.现代塑料加工应用，第11卷第3期. 1999 |
| 超高分子量聚乙烯冻胶纤维的制备. 尹德荟，李炳海等.现代塑料加工应用，第11卷第3期. 1999 * |
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Assignee: Jiangsu Shentai Science & Technology Development Co., Ltd. Assignor: Donghua University Contract fulfillment period: 2009.1.28 to 2017.1.28 contract change Contract record no.: 2009320000265 Denomination of invention: Prepn and application of jelly fiber of polyethylene in ultrahigh molecular weight Granted publication date: 20081022 License type: Exclusive license Record date: 2009.3.10 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.1.28 TO 2017.1.28; CHANGE OF CONTRACT Name of requester: JIANGSU SHENTAI TECHNOLOGY DEVELOPMENT CO., LTD. Effective date: 20090310 |
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Granted publication date: 20081022 Termination date: 20161124 |
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