The preparation method of high concentration ultra-high molecular weight polyethylene spinning solution
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 properties, becomes the third generation high-performance fiber occurring after carbon fiber and aramid fiber.With regard to intensity, at present can the sling maximum weight come 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 industrialized fiber at present.In addition, the density of superhigh molecular weight polyethylene fibers is less than carbon fiber and aramid fiber, has excellent chemical resistance and weather fastness, high-energy absorption, low electric conductivity, the features such as water proofing property.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, after improving, level further improves, and to the mid-90, production scale has reached 1000t/.Only have in the world at present Dutch DSM N. V., Allied company of the U.S., the production that company and Deng Ji company of Mitsui have patented technology and formed industrially scalable is spun by Japanese Japan.
The manufacture of domestic superhigh molecular weight polyethylene fibers is in the stage that limit produces, limit is groped, improve on limit, limit is perfect, during having, main manufacturing enterprise spins investment Beijing with Yi Zhong special fibre company (1200 tons of annual productions), Ningbo Dacheng New Material Co., Ltd (1200 tons of left and right of annual production), and Hunan Zhong Tai company (1200 tons of left and right of annual production).And due to the wilderness demand of international market, domestic manufacturer is all constantly being expanded or plan expands its production scale, the demand of, international market domestic to adapt to.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 comprising with ultra-high molecular weight polyethylene and solubilized ultra-high molecular weight polyethylene, prepare the method for super high molecular polyethylene solution through swelling and dissolving, improve the uniformity of solution and the method for shortening dissolution time, and improve the tensile property of gel spun fiber.Chinese patent 01123737.6 also discloses a kind of manufacture method of superhigh molecular weight polyethylene fibers, the parameters such as aperture, draw ratio and the rate of extrusion of the molecular weight that utilizes semi-enclosed temperature-controlled area and coupling, original liquid concentration, spinneret orifice, by regulating the longitudinal stretching speed after spinning solution or spinning melt are extruded, part macromolecule entanglement point is removed, obtain having the precursor of suitable supramolecular structure, obtain superhigh molecular weight polyethylene fibers through multistage stretching processing.But above technique is all mentioned the solid content that improves spinning solution, to enhance productivity.
Chinese patent 200810034216.4 and Chinese patent 200810034215.X disclose respectively the spinning technique of superhigh molecular weight polyethylene fibers, adopt the continuous processing that one-step method is swelling and dissolve, spinning solution concentration is brought up to 10 ~ 15% by original 5 ~ 8%, and production efficiency improves more than 30%.But in described technique, do not mention the control problem of molecular weight degradation in production process.
Chinese patent 101775666 discloses a kind of preparation method of high concentration superhigh molecular weight polyethylene fibers, first the super high molecular weight polyethylene gel that a kind of concentration is 1 ~ 10%, then frozen glue is ground into the particle of 0.1mm ~ 30mm, obtaining solid content through supercentrifuge de-oiling is that 20% ~ 70% ultra-high molecular weight polyethylene is original, feeding double screw extruder extruding spinning, through extraction, dry and super doubly hot drawing-off, obtain superhigh molecular weight polyethylene fibers.But, due to operations such as many preparations of low concentration frozen glue, cooling, pulverizing and de-oilings, the advantage of high concentration is not not fully exerted.
Summary of the invention
The object of the present invention is to provide a kind of production process intermediate link, preparation method of the high concentration ultra-high molecular weight polyethylene spinning solution of enhancing productivity of reducing.
Technical solution of the present invention is:
A preparation method for 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 joins in solvent together with antioxidant by 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), by the super high molecular polyethylene solution of low concentration concentration at 190 ~ 220 DEG C, obtain even, consoluet 10% ~ 20% high concentration super high molecular polyethylene solution.
In step (1), mixing speed is 80 ~ 100 revs/min; Dissolving refers to dissolves 4 ~ 8 hours under the high temperature of 190 ~ 220 DEG C.
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 irgasfos 168, 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, first ultra-high molecular weight polyethylene is fully dissolved, then improve spinning concentration by high temperature centrifugal concentrating, the uniform consoluet spinning solution of final preparation, for the superhigh molecular weight polyethylene fibers of the high-quality precursor of follow-up preparation and high-quality lays the foundation.
The invention has the beneficial effects as follows:
1, reduce the loaded down with trivial details operation of configuration spinning solution, increase work efficiency;
2, improve spinning solution concentration, improve twin-screw extrusion efficiency;
3, can prepare uniform consoluet spinning solution, for the superhigh molecular weight polyethylene fibers of the high-quality precursor of follow-up 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 invention will be further described.
Detailed description of the invention
A preparation method for 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 joins in solvent together with antioxidant by molecular weight, the mass percent of ultra-high molecular weight polyethylene, antioxidant and solvent is 2 ~ 3:0.0025 ~ 0.04:100(example 2:0.025:100,2.5:0.03:100,3:0.04:100), stir on dissolving limit, limit, high-temperature digestion, makes the super high molecular polyethylene solution of low concentration;
(2) by the ultra-high molecular weight polyethylene pyrosol of low concentration concentration under 190 ~ 220 DEG C (190 DEG C, 210 DEG C, 220 DEG C of examples), obtain even, consoluet 10% ~ 20%(example 10%, 15%, 20%) high concentration super high molecular polyethylene solution.
In step (1), stir speed (S.S.) is 80 ~ 100 revs/min; High-temperature digestion is under the high temperature of 190 ~ 220 DEG C (190 DEG C, 210 DEG C, 220 DEG C of examples), to dissolve 4 ~ 8 hours (example 4 hours, 6 hours, 8 hours).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 (example 10 orders, 30 orders, 60 orders).Described solvent is white oil or kerosene.Described antioxidant is a kind of in irgasfos 168, antioxidant 1010 or two kinds.