CN101153079B - Method of preprocessing ultrahigh molecular weight polyethylene for spinning - Google Patents
Method of preprocessing ultrahigh molecular weight polyethylene for spinning Download PDFInfo
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- CN101153079B CN101153079B CN200610116781A CN200610116781A CN101153079B CN 101153079 B CN101153079 B CN 101153079B CN 200610116781 A CN200610116781 A CN 200610116781A CN 200610116781 A CN200610116781 A CN 200610116781A CN 101153079 B CN101153079 B CN 101153079B
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Abstract
The present invention relates to a pretreatment method of polyethylene of ultra-high molecular weight for spinning. The method comprises the following process steps: the polyethylene powder of ultra-high molecular weight and composite solvent are added into a dissolution kettle according to a weight ratio of 0.01 to 0.5: 1; the mixture is stirred for 1 to 60 minutes at a temperature of 50 to 150 DEG C and then filtered; the secondary solvent is then used for cleaning and filtering to prepare the polyethylene of ultra-high molecular weight for spinning. Compared with the prior art, the present invention has the characteristics that the molecular weight distribution of the polyethylene of ultra-high molecular weight is narrowed so as to get fiber of higher strength, strength, modulus and creeping resistance in spinning.
Description
Technical field
The present invention relates to a kind of poly pretreatment process, relate in particular to the pretreatment process of the special-purpose ultrahigh molecular weight polyethylene(UHMWPE) of a kind of spinning.
Background technology
Ultrahigh molecular weight polyethylene(UHMWPE) (UHMWPE) fiber is a kind of to have high strength, a high-modulus high-performance fiber by average molecular mass what the polyethylene more than 1,000,000 spinning formed, in addition, it also has excellent chemical resistant properties and weathering resistance, high-energy absorption, low electric conductivity, can see through X-ray and certain characteristics such as water-repellancy.The performance that this fiber is outstanding makes it in military affairs, space flight navigation engineering and high-performance, light weight matrix material, and sports movement apparatus, there is wide application prospect in fields such as biomaterial.
DSM N. V. of Holland in 1979 at first discloses the patent (NL7900990 of gel spinning spinning UHMWPE fiber, NL7904990 and corresponding US4344908, special public clear 64-8732, US4422993), it is solvent that U.S.'s allied signal (Allied-Singal) company has developed with kerosene or white oil on this basis, Freon 113 (Refrigerant R 113) is the wet method gel spinning technology (US430577 of extraction agent, special fair 1-16924, EP0064167, EP0205960), still can not satisfy the application scenario that thinner requirement is arranged for fiber.Japan spins company and has bought DSM N. V.'s patent, and reach the industrialization development cooperation agreement with DSM N. V., develop jointly with the perhydronaphthalene is that (spy opens flat 4-209817 for the dry method gel spinning industrialization technology of solvent, Te Kaiping 7-166414), its filament number only reaches 2d, still can not satisfy the application scenario that thinner requirement is arranged for fiber.
Domestic research and the industrialization development work that has how tame research unit to carry out kerosene, white oil, paraffin or paraffin oil, perhydronaphthalene equal solvent system UHMWPE in succession, wherein successful is that China Textile University is first solvent with kerosene or white oil, is the wet method gel spinning technology (CN1056544A) of second extraction solvent with gasoline.
But the UHMWPE fiber of domestic production at present all exists fiber surface to send out the scared defective of suede, and intensity, modulus and the creep resistance of fiber are restricted, and can not satisfy the service requirements of high-performance fiber.The major cause that causes this phenomenon is because used UHMWPE molecular weight distribution compares broad, in the process that the PE sheet crystal orientation uncrimping chain that super times thermal stretch is a folded chain transforms, the molecule segment of low molecular weight part is broken easily, makes fiber surface that the scared phenomenon of suede of sending out be arranged.
Summary of the invention
Purpose of the present invention is exactly the pretreatment process that the ultrahigh molecular weight polyethylene for spinning of a kind of high strength, modulus and creep resistance fiber is provided for the weak point that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of pretreatment process of ultrahigh molecular weight polyethylene for spinning, it is characterized in that, this method comprises following processing step: ultrahigh molecular weight polyethylene(UHMWPE) powder and double solvents are (0.01～0.5) by weight: 1 ratio joins in the dissolution kettle, at 1～60 minute after-filtration of 50～150 ℃ of following stirring and dissolving, filter with second solvent cleaning then, make ultrahigh molecular weight polyethylene for spinning.
The weight ratio of described ultrahigh molecular weight polyethylene(UHMWPE) powder and double solvents is: (0.05～0.3): 1.
The molecular-weight average of described ultrahigh molecular weight polyethylene(UHMWPE) powder is at 400-700 ten thousand.
How described double solvents is selected from decahydro, one or more composite the forming in paraffin oil or the kerosene.
The volume of described dissolution kettle is 50～100L.
Described solvent temperature is 90～135 ℃.
Described dissolution time is 2～30 minutes.
Described second solvent comprises hexane or toluene.
Compared with prior art, the present invention is by removing the UHMWPE low molecular weight part, the molecular weight distribution of UHMWPE is narrowed down, thereby can obtain UHMWPE fiber high-strength, Gao Mo, the preparation method of the special-purpose ultrahigh molecular weight polyethylene(UHMWPE) of this gel spinning, make intensity, modulus and the creep resistance of fiber unrestricted, satisfy the service requirements of high-performance fiber, solved fiber surface and sent out the scared defective of suede.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
With 20 parts of viscosity-average molecular weights is that 5,500,000 UHMWPE powder, 80 parts perhydronaphthalene and the mixed solvent (weight ratio of perhydronaphthalene and paraffin oil is 1: 3) of paraffin oil are put into dissolution kettle, be rapidly heated while stirring to 110 ℃, stirred 5 minutes at 110 ℃, filter then, with the UHMWPE powder after filtering with 40 ℃ hexane cleaning and filtering 3 times.
It is 5,730,000 that the UHMWPE powder that cleaning and filtering is good records viscosity-average molecular weight with GB 1841-80 (polyolefin resin dilute solution viscosity test method).
Embodiment 2
With 5 parts of viscosity-average molecular weights is that 7,000,000 UHMWPE powder, 95 parts perhydronaphthalene and the mixed solvent (weight ratio of perhydronaphthalene and paraffin oil is 1: 5) of paraffin oil are put into dissolution kettle, be rapidly heated while stirring to 135 ℃, stirred 20 minutes at 135 ℃, filter then, with the UHMWPE powder after filtering with 60 ℃ toluene cleaning and filtering 3 times.
It is 7,410,000 that the UHMWPE powder that cleaning and filtering is good records viscosity-average molecular weight with GB 1841-80 (polyolefin resin dilute solution viscosity test method).
Embodiment 3
With 30 parts of viscosity-average molecular weights is that 4,000,000 UHMWPE powder, 70 parts perhydronaphthalene and the mixed solvent (weight ratio of perhydronaphthalene and paraffin oil is 1: 3) of paraffin oil are put into dissolution kettle, be rapidly heated while stirring to 90 ℃, stirred 30 minutes at 90 ℃, filter then, with the UHMWPE powder after filtering with 60 ℃ toluene cleaning and filtering 3 times.
It is 4,570,000 that the UHMWPE powder that cleaning and filtering is good records viscosity-average molecular weight with GB 1841-80 (polyolefin resin dilute solution viscosity test method).
Embodiment 4
With 15 parts of viscosity-average molecular weights is that 6,000,000 UHMWPE powder, 85 parts perhydronaphthalene and the mixed solvent (weight ratio of perhydronaphthalene and kerosene is 1: 4) of kerosene are put into dissolution kettle, be rapidly heated while stirring to 115 ℃, stirred 15 minutes at 115 ℃, filter then, with the UHMWPE powder after filtering with 60 ℃ toluene cleaning and filtering 3 times.
It is 6,390,000 that the UHMWPE powder that cleaning and filtering is good records viscosity-average molecular weight with GB 1841-80 (polyolefin resin dilute solution viscosity test method).
Claims (6)
1. the pretreatment process of a ultrahigh molecular weight polyethylene for spinning, it is characterized in that, this method comprises following processing step: ultrahigh molecular weight polyethylene(UHMWPE) powder and double solvents are (0.01～0.5) by weight: 1 ratio joins in the dissolution kettle, at 1～60 minute after-filtration of 50～150 ℃ of following stirring and dissolving, filter with second solvent cleaning then, make ultrahigh molecular weight polyethylene for spinning; Described double solvents is selected from one or more composite the forming in perhydronaphthalene, paraffin oil or the kerosene; Described second solvent is hexane or toluene.
2. the pretreatment process of a kind of ultrahigh molecular weight polyethylene for spinning according to claim 1 is characterized in that, the weight ratio of described ultrahigh molecular weight polyethylene(UHMWPE) powder and double solvents is: (0.05～0.3): 1.
3. the pretreatment process of a kind of ultrahigh molecular weight polyethylene for spinning according to claim 1 is characterized in that, the viscosity-average molecular weight of described ultrahigh molecular weight polyethylene(UHMWPE) powder is 4,000,000-7,000,000.
4. the pretreatment process of a kind of ultrahigh molecular weight polyethylene for spinning according to claim 1 is characterized in that, the volume of described dissolution kettle is 50～100L.
5. the pretreatment process of a kind of ultrahigh molecular weight polyethylene for spinning according to claim 1 is characterized in that, described solvent temperature is 90～135 ℃.
6. the pretreatment process of a kind of ultrahigh molecular weight polyethylene for spinning according to claim 1 is characterized in that, described dissolution time is 2～30 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610116781A CN101153079B (en) | 2006-09-29 | 2006-09-29 | Method of preprocessing ultrahigh molecular weight polyethylene for spinning |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610116781A CN101153079B (en) | 2006-09-29 | 2006-09-29 | Method of preprocessing ultrahigh molecular weight polyethylene for spinning |
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| CN101153079A CN101153079A (en) | 2008-04-02 |
| CN101153079B true CN101153079B (en) | 2010-05-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0255618A2 (en) * | 1986-07-08 | 1988-02-10 | Nippon Petrochemicals Co., Ltd. | Ultra-high-molecular-weight polyethylene solution |
| CN1240798A (en) * | 1998-07-07 | 2000-01-12 | 南京大学 | Process for improving flowability of linear low-density polyethylene resin in processing |
| CN1405367A (en) * | 2001-08-13 | 2003-03-26 | 中纺投资发展股份有限公司 | Method for preparing extra high molecular polyethylene high-concentrated solution for spinning |
| CN1631943A (en) * | 2004-11-29 | 2005-06-29 | 北京特斯顿新材料技术发展有限公司 | Method for continuous preparation and mixture of super high molecular polyethylene solution |
-
2006
- 2006-09-29 CN CN200610116781A patent/CN101153079B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0255618A2 (en) * | 1986-07-08 | 1988-02-10 | Nippon Petrochemicals Co., Ltd. | Ultra-high-molecular-weight polyethylene solution |
| CN1240798A (en) * | 1998-07-07 | 2000-01-12 | 南京大学 | Process for improving flowability of linear low-density polyethylene resin in processing |
| CN1405367A (en) * | 2001-08-13 | 2003-03-26 | 中纺投资发展股份有限公司 | Method for preparing extra high molecular polyethylene high-concentrated solution for spinning |
| CN1631943A (en) * | 2004-11-29 | 2005-06-29 | 北京特斯顿新材料技术发展有限公司 | Method for continuous preparation and mixture of super high molecular polyethylene solution |
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| CN101153079A (en) | 2008-04-02 |
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Address after: 201512 Jinshan District Jinshan Road, Shanghai, No. 4480 Co-patentee after: Shanghai Chemical Research Institute Co., Ltd. Patentee after: Shanghai Chemical Institute Tiandi Technology Development Co., Ltd. Co-patentee after: Shanghai Lianle Chemical Industry Science and Technology Co., Ltd. Address before: 201512 Jinshan District Jinshan Road, Shanghai, No. 4480 Co-patentee before: Shanghai Research Institute of Chemical Industry Patentee before: Shanghai Chemical Institute Tiandi Technology Development Co., Ltd. Co-patentee before: Shanghai Lianle Chemical Industry Science and Technology Co., Ltd. |