CN102605440A - High-concentration superhigh-molecular-weight polyethylene spinning solution preparation method - Google Patents
High-concentration superhigh-molecular-weight polyethylene spinning solution preparation method Download PDFInfo
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Abstract
The invention discloses a high-concentration superhigh-molecular-weight polyethylene spinning solution preparation method, which includes steps of adding 5-8 million parts of superhigh-molecular-weight polyethylene powder and oxidation inhibitor into solution, dissolving at the high temperature, obtaining low-concentration superhigh-molecular-weight polyethylene solution; concentrating the low-concentration superhigh-molecular-weight high-temperature polyethylene solution at the temperature of 190-220 DEG C, and obtaining uniform totally-dissolved superhigh-molecular-weight polyethylene solution with high concentration of 10-20%. By the high-concentration superhigh-molecular-weight polyethylene spinning solution preparation method, intermediate links during production are reduced, production efficiency is improved and production cost is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of high concentration ultra-high molecular weight polyethylene spinning solution.
Background technology
Superhigh molecular weight polyethylene fibers has excellent physical and mechanical performance, becomes the third generation high-performance fiber that after carbon fiber and aramid fiber, occurs.With regard to intensity, at present can the sling maximum weight of coming of superhigh molecular weight polyethylene fibers rope is the octuple of the same thickness steel wire rope maximum weight of slinging, and is the highest fiber of intensity in the industrialized fiber at present.In addition, the density of superhigh molecular weight polyethylene fibers has excellent chemical resistance and weather fastness, high-energy absorption property, low electric conductivity, characteristics such as water proofing property less than carbon fiber and aramid fiber.In view of above-mentioned performance, this fiber becomes another main high-performance fiber after carbon fiber and aramid fiber.Dutch DSM N. V. in 1979 have applied for the production patent of this fiber first; Allied-signal Inc. (US) Columbia Road and Park Avenue, Morris Township, Morris C of the U.S. (present Honeywell company) has bought this patent subsequently; Level further improves after improving, and to the mid-90, production scale has reached 1000t/.Have only Dutch DSM N. V. at present in the world, the production that several companies such as company and Mitsui have patented technology and formed industrially scalable is spun by U.S. Allied company, Japanese Japan.
The manufactureization of domestic superhigh molecular weight polyethylene fibers is in the stage that the limit produces, the limit is groped, improve on the limit, the limit is perfect; During having, main manufacturing enterprise spins investment Beijing with special fibre company in the benefit (1200 tons of annual productions); Safe company (about 1200 tons of annual productions) in Ningbo Dacheng New Material Co., Ltd's (about 1200 tons of annual productions) and the Hunan.And because the wilderness demand of international market, make domestic manufacturer all constantly enlarge or plan enlarges its production scale, the demand of, international market domestic to adapt to.The superhigh molecular weight polyethylene fibers industry is in the industry growth stage at present, and development prospect is wide.
Chinese patent 89107905.X discloses a kind of organic solvent that comprises with ultra-high molecular weight polyethylene and solubilized ultra-high molecular weight polyethylene; The method for preparing super high molecular polyethylene solution through swelling and dissolving; Improve the uniformity and the method that shortens dissolution time of solution, and improve the tensile property of gel spun fiber.Chinese patent 01123737.6 also discloses a kind of manufacturing approach of superhigh molecular weight polyethylene fibers; Be the parameters such as aperture, draw ratio and rate of extrusion of the molecular weight that utilizes semi-enclosed temperature-controlled area and coupling, original liquid concentration, spinneret orifice; Through regulating the longitudinal stretching speed after spinning solution or spinning melt are extruded; Part macromolecule entanglement point is removed, and the precursor that obtains having suitable supramolecular structure obtains superhigh molecular weight polyethylene fibers through the multistage stretching processing.But above technology is all mentioned the solid content that improves spinning solution, to enhance productivity.
Chinese patent 200810034216.4 and Chinese patent 200810034215.X disclose the spinning technique of superhigh molecular weight polyethylene fibers respectively; Adopt the continuous processing of one-step method swelling and dissolving; Spinning solution concentration is brought up to 10 ~ 15% by original 5 ~ 8%, and production efficiency improves more than 30%.But do not mention the control problem of molecular weight degradation in the production process in the said technology.
Chinese patent 101775666 discloses a kind of preparation method of high concentration superhigh molecular weight polyethylene fibers; At first a kind of concentration is 1 ~ 10% super high molecular weight polyethylene gel; Then frozen glue is ground into the particle of 0.1mm ~ 30mm, obtaining solid content through the supercentrifuge de-oiling is that 20% ~ 70% ultra-high molecular weight polyethylene is original, feeding double screw extruder extruding spinning; Through extraction, dry and ultra doubly hot drawing-off, obtain superhigh molecular weight polyethylene fibers.But, because many operations such as preparation, cooling, pulverizing and de-oiling of low concentration frozen glue make the advantage of high concentration not be not fully exerted.
Summary of the invention
The object of the present invention is to provide a kind of minimizing production process intermediate link, the preparation method of the high concentration ultra-high molecular weight polyethylene spinning solution of enhancing productivity.
Technical solution of the present invention is:
A kind of preparation method of high concentration ultra-high molecular weight polyethylene spinning solution is characterized in that: comprise the following steps:
(1) be that 5,000,000 to 8,000,000 ultra-high molecular weight polyethylene powder and antioxidant join in the solvent together with molecular weight; The mass percent of ultra-high molecular weight polyethylene, antioxidant and solvent is 2 ~ 3:0.0025 ~ 0.04:100; Dissolve while stirring, make the super high molecular polyethylene solution of low concentration;
(2) with the super high molecular polyethylene solution of low concentration 190 ~ 220 ℃ of following concentration, obtain even, consoluet 10% ~ 20% high concentration super high molecular polyethylene solution.
Mixing speed is 80 ~ 100 rev/mins in the step (1); Dissolving is meant under 190 ~ 220 ℃ high temperature dissolved 4 ~ 8 hours.
Step (2) the concentration time is 8 ~ 10 minutes.
Described ultra-high molecular weight polyethylene powder diameter is 10 ~ 60 orders.
Described solvent is white oil or kerosene.
Described antioxidant is a kind of in antioxidant 168, the antioxidant 1010 or two kinds.
The invention provides a kind of preparation method of high concentration ultra-high molecular weight polyethylene spinning solution; It is a kind of easy process route; At first fully dissolve ultra-high molecular weight polyethylene; Through the centrifugal concentrated raising spinning concentration of high temperature, finally prepare uniform consoluet spinning solution then, for the high-quality precursor of subsequent preparation and high-quality superhigh molecular weight polyethylene fibers lay the foundation.
The invention has the beneficial effects as follows:
1, reduces the loaded down with trivial details operation of configuration spinning solution, increase work efficiency;
2, improve spinning solution concentration, improve the twin-screw extrusion efficiency;
3, can prepare uniform consoluet spinning solution, for the superhigh molecular weight polyethylene fibers of high-quality precursor of subsequent preparation and high strength and modulus lays the first stone;
4, reduce using and consuming of solvent and extractant, energy-conserving and environment-protective reduce production costs.
Below in conjunction with embodiment the present invention is described further.
The specific embodiment
A kind of preparation method of high concentration ultra-high molecular weight polyethylene spinning solution comprises the following steps:
(1) be that 5,000,000 to 8,000,000 ultra-high molecular weight polyethylene powder and antioxidant join in the solvent together with molecular weight; The mass percent of ultra-high molecular weight polyethylene, antioxidant and solvent is 2 ~ 3:0.0025 ~ 0.04:100 (routine 2:0.025:100,2.5:0.03:100,3:0.04:100); Stir while dissolving; High-temperature digestion makes the super high molecular polyethylene solution of low concentration;
(2) with ultra-high molecular weight polyethylene pyrosol concentration under 190 ~ 220 ℃ (190 ℃, 210 ℃, 220 ℃ of examples) of low concentration, obtain even, consoluet 10% ~ 20% (example 10%, 15%, 20%) high concentration super high molecular polyethylene solution.
Stir speed (S.S.) is 80 ~ 100 rev/mins in the step (1); High-temperature digestion is dissolving 4 ~ 8 hours (example 4 hours, 6 hours, 8 hours) under the high temperature of 190 ~ 220 ℃ (190 ℃, 210 ℃, 220 ℃ of examples).Step (2) the concentration time is 8 ~ 10 minutes (example 8,9,10 minutes).
Described ultra-high molecular weight polyethylene powder diameter is 10 ~ 60 orders (routine 10 orders, 30 orders, 60 orders).Described solvent is white oil or kerosene.Described antioxidant is a kind of in antioxidant 168, the antioxidant 1010 or two kinds.
Claims (6)
1. the preparation method of a high concentration ultra-high molecular weight polyethylene spinning solution is characterized in that: comprise the following steps:
(1) be that 5,000,000 to 8,000,000 ultra-high molecular weight polyethylene powder and antioxidant join in the solvent together with molecular weight; The mass percent of ultra-high molecular weight polyethylene, antioxidant and solvent is 2 ~ 3:0.0025 ~ 0.04:100; Dissolve while stirring, make the super high molecular polyethylene solution of low concentration;
(2) with the super high molecular polyethylene solution of low concentration 190 ~ 220 ℃ of following concentration, obtain even, consoluet 10% ~ 20% high concentration super high molecular polyethylene solution.
2. the preparation method of high concentration ultra-high molecular weight polyethylene spinning solution according to claim 1 is characterized in that: stir speed (S.S.) is 80 ~ 100 rev/mins in the step (1); High-temperature digestion is under 190 ~ 220 ℃ high temperature, to dissolve 4 ~ 8 hours.
3. the preparation method of high concentration ultra-high molecular weight polyethylene spinning solution according to claim 1 is characterized in that: step (2) the concentration time is 8 ~ 10 minutes.
4. according to the preparation method of claim 1,2 or 3 described high concentration ultra-high molecular weight polyethylene spinning solutions, it is characterized in that: described ultra-high molecular weight polyethylene powder diameter is 10 ~ 60 orders.
5. according to the preparation method of claim 1,2 or 3 described high concentration ultra-high molecular weight polyethylene spinning solutions, it is characterized in that: described solvent is white oil or kerosene.
6. according to the preparation method of claim 1,2 or 3 described high concentration ultra-high molecular weight polyethylene spinning solutions, it is characterized in that: described antioxidant is a kind of in antioxidant 168, the antioxidant 1010 or two kinds.
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| CN102605440B CN102605440B (en) | 2014-11-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158160A (en) * | 2019-06-28 | 2019-08-23 | 上海化工研究院有限公司 | A kind of method of high concentration gel spinning preparation ultra high molecular weight polyethylene fiber |
| CN110658036A (en) * | 2019-09-05 | 2020-01-07 | 上海化工研究院有限公司 | Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution |
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| EP0255109A2 (en) * | 1986-07-28 | 1988-02-03 | Mitsubishi Rayon Co., Ltd. | Process for producing an acrylic fiber having high fiber characteristics |
| CN101492285A (en) * | 2009-03-11 | 2009-07-29 | 中南大学 | Process for producing fibre containing beryllium |
| CN101775666A (en) * | 2010-01-22 | 2010-07-14 | 东华大学 | Preparation method of high-strength high-modulus polyethylene fiber |
| CN102358956A (en) * | 2011-07-21 | 2012-02-22 | 金云良 | Method for preparing high-strength and high-modulus polyethylene fiber |
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2012
- 2012-03-29 CN CN201210087466.0A patent/CN102605440B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0255109A2 (en) * | 1986-07-28 | 1988-02-03 | Mitsubishi Rayon Co., Ltd. | Process for producing an acrylic fiber having high fiber characteristics |
| CN101492285A (en) * | 2009-03-11 | 2009-07-29 | 中南大学 | Process for producing fibre containing beryllium |
| CN101775666A (en) * | 2010-01-22 | 2010-07-14 | 东华大学 | Preparation method of high-strength high-modulus polyethylene fiber |
| CN102358956A (en) * | 2011-07-21 | 2012-02-22 | 金云良 | Method for preparing high-strength and high-modulus polyethylene fiber |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158160A (en) * | 2019-06-28 | 2019-08-23 | 上海化工研究院有限公司 | A kind of method of high concentration gel spinning preparation ultra high molecular weight polyethylene fiber |
| CN110158160B (en) * | 2019-06-28 | 2024-02-27 | 上海化工研究院有限公司 | Method for preparing ultra-high molecular weight polyethylene fiber by high-concentration gel spinning |
| CN110658036A (en) * | 2019-09-05 | 2020-01-07 | 上海化工研究院有限公司 | Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution |
| CN110658036B (en) * | 2019-09-05 | 2022-05-06 | 上海化工研究院有限公司 | Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution |
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| CN102605440B (en) | 2014-11-26 |
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Address after: 226407 the Yellow Sea three road, Nantong Economic Development Zone, Rudong County, Jiangsu, China Patentee after: Jiangsu BICON Pharmaceutical Co., Ltd. Patentee after: Jiangsu Shentai Science & Technology Development Co., Ltd. Address before: 226407 the Yellow Sea three road, Nantong Economic Development Zone, Rudong County, Jiangsu, China Patentee before: Jiangsu Jiujiujiu Technology Co., Ltd. Patentee before: Jiangsu Shentai Science & Technology Development Co., Ltd. |
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