CN101736431A - Production method of high-strength high-modulus PMIA super-short fiber - Google Patents
Production method of high-strength high-modulus PMIA super-short fiber Download PDFInfo
- Publication number
- CN101736431A CN101736431A CN200910259778A CN200910259778A CN101736431A CN 101736431 A CN101736431 A CN 101736431A CN 200910259778 A CN200910259778 A CN 200910259778A CN 200910259778 A CN200910259778 A CN 200910259778A CN 101736431 A CN101736431 A CN 101736431A
- Authority
- CN
- China
- Prior art keywords
- modulus
- pmia
- super
- short fiber
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a preparation method of high-strength high-modulus PMIA super-short fiber, comprising: m-phthaloyl chloride and metaphenylene diamine are adopted in a system of which the sulphonamide compound is an organic solvent to polymerize solution to obtain m-phenyleneisophthalamide (PMIA) solution comprising polymetaphenylene isophthamide as a repeating unit; performing neutralization reaction by calcium oxide or calcium hydroxide to generate hydrochloric acid so as to obtain spinning solution, wherein the logarithmic viscosity number of the spinning solution is 3-6; high-strength high-modulus PMIA super-short fiber of which the length is 0.5-20 mm is prepared by wet spinning, cleaning, heat treatment, winding, cutting off and packaging. The strength and the modulus of the PMIA super-short fiber are greatly improved compared with the existing like products.
Description
Technical field
The invention belongs to the aramid fiber preparation field, particularly the high-strength high-modulus PMIA super-short fiber preparation method.
Background technology
Aramid fiber (Aramid fiber) is a kind of novel high-tech synthetic fiber, mainly be divided into two kinds, a contraposition aramid fiber (PPTA) and a position aramid fiber (PMIA) have superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, premium properties such as in light weight, and its intensity is 5～6 times of steel wire, modulus is steel wire or glass fibre 2～3 times, toughness is 2 times of steel wire, and weight only is about 1/5 of steel wire, under 560 ℃ temperature, do not decompose, do not melt.It has good insulation performance and ageing resistace, has very long life cycle.The discovery of aramid fiber is considered to very important historical progress of material circle.The meta-aramid superbhort fiber is to produce one of used main raw material of aramid fiber paper, is with a wide range of applications, and the intensity and the modulus of the aramid fiber paper that present common meta-aramid superbhort fiber is produced are all undesirable.
Summary of the invention
The object of the invention is to provide the production method of the aramid fiber superbhort fiber of a kind of high strength and high film amount.
The preparation method of high-strength high-modulus PMIA super-short fiber of the present invention, comprising following steps:
In the system that with the amide compound is organic solvent, carry out polymerisation in solution with m-phthaloyl chloride and m-phenylene diamine (MPD), obtain comprising the meta-aromatic polyamide solution that mpd-i is a repetitive, carry out the hydrochloric acid that neutralization reaction generates with calcium oxide or calcium hydroxide, get spinning solution, the logarithmic viscosity number that makes spinning solution is at 3-6;
Promptly get through wet spinning, cleaning, heat treatment, coiling, cut-out, packing and to make the high-strength high-modulus PMIA super-short fiber that length is the 0.5-20 millimeter.
The preparation method of high-strength high-modulus PMIA super-short fiber of the present invention, wherein wet spinning is to be that the spinning head of the spinneret orifice of 0.01-2 millimeter is extruded with the spinning solution deaeration and by diameter, form long filament in temperature is 20-50 ℃ aqueous coagulation bath, drawing-off doubly makes it have the certain physical mechanical performance through 2-10 in containing calcium chloride water.
The preparation method of high-strength high-modulus PMIA super-short fiber of the present invention, wherein heat treatment step is, is to carry out high-temperature shaping under 350-450 ℃ at setting temperature.
The preparation method of high-strength high-modulus PMIA super-short fiber of the present invention, wherein amide compound is selected from dimethyl formamide or dimethylacetylamide.
The present invention once adds m-phthaloyl chloride in the polymerisation time-division, and only once neutralization is controlled the logarithmic viscosity number of rational stoste, the size of drawing-off, heat treated condition, thereby made the aramid fiber superbhort fiber that makes have higher intensity and modulus.
The present invention will be further described below by the specific embodiment.
The specific embodiment
Embodiment 1
1, in the solution of dimethylacetylamide, carries out polymerisation in solution, carry out the hydrochloric acid that neutralization reaction generates, get spinning solution with calcium hydroxide with monomer m-phthaloyl chloride (IPC) and monomer m-phenylene diamine (MPD) (MPDA);
The spinning solution that adopts before the wet spinning is the less salt spinning solution, carry out the polymerisation time-division and once add m-phthaloyl chloride, once neutralization, by the addition and the suitable terminator of adding of control m-phthaloyl chloride, the logarithmic viscosity number that makes spinning solution is 4.3-4.6.
2, wet spinning: is in the spinneret orifice of 0.01-2 millimeter to extrude by diameter with spinning solution after deaeration, by temperature is that 20 ℃ the aqueous solution forms long filament, through a kind of special drawing machine in a kind of aqueous solution that contains calcium chloride, drawing-off makes it have the favorable mechanical performance for 2 times, washing, drying fibrous;
3, the product after the oven dry is carried out 350 ℃ of heat treatments, further improve the mechanical performance of fiber;
4, become high-strength and high-modulus meta-aramid endless tow through the fiber after the Overheating Treatment behind the coiling winder, re-use special cutting machine and cut off, the staple length after the cut-out is generally between the 0.5-20 millimeter, after screening, and packing and binding.
Embodiment 2
1, in the solution of dimethyl formamide, carries out polymerisation in solution, carry out the hydrochloric acid that neutralization reaction generates, get spinning solution with calcium oxide with monomer m-phthaloyl chloride (IPC) and monomer m-phenylene diamine (MPD) (MPDA); The logarithmic viscosity number of spinning solution is 4.6-4.9.
2, wet spinning: is that the spinneret orifice of 0.01-2 millimeter heavily extrude by diameter with spinning solution after deaeration, by temperature is that 40 ℃ the aqueous solution forms long filament, through a kind of special drawing machine in a kind of aqueous solution that contains calcium chloride, drawing-off makes it have the favorable mechanical performance for 6 times, washing, drying fibrous;
3, the product after the oven dry is carried out 400 ℃ of heat treatments;
4, become high-strength and high-modulus meta-aramid endless tow through the fiber after the Overheating Treatment behind the coiling winder, re-use special cutting machine and cut off, the staple length after the cut-out is generally between the 0.5-20 millimeter, after screening, and packing and binding.
Embodiment 3
1, in the solution of dimethylacetylamide, carries out polymerisation in solution, carry out the hydrochloric acid that neutralization reaction generates, get spinning solution with calcium hydroxide with monomer m-phthaloyl chloride (IPC) and monomer m-phenylene diamine (MPD) (MPDA); The logarithmic viscosity number of spinning solution is 5.4-5.7.
2, wet spinning: is that the spinneret orifice of 0.01-2 millimeter heavily extrude by diameter with spinning solution after deaeration, by temperature is that 50 ℃ the aqueous solution forms long filament, through a kind of special drawing machine in a kind of aqueous solution that contains calcium chloride, drawing-off makes it have the favorable mechanical performance for 10 times, washing, drying fibrous;
3, the product after the oven dry is carried out 450 ℃ of heat treatments, further improve the mechanical performance of fiber;
4, become high-strength and high-modulus meta-aramid endless tow through the fiber after the Overheating Treatment behind the coiling winder, re-use special cutting machine and cut off, the staple length after the cut-out is generally between the 0.5-20 millimeter, after screening, and packing and binding.
Can learn from the result of above-mentioned each embodiment, the logarithmic viscosity number of stoste, the size of drawing-off and heat treated effect have determined the intensity and the modulus of fiber, experimental results show that, the physical and mechanical properties of fiber and above-described several factor corresponding relation in direct ratio, but can not be excessive, after the value of reaching capacity, the performance of fiber can reduce.The test result of the high-strength high-modulus fibre of common meta-aramid fibers and present embodiment 1 is seen contrast table 1, and the high-strength and high-modulus staple fiber has better solved fiber dispersion inequality in the paper process, shortcomings such as product strength difference.The practical efficiency of staple fiber improves 10%, surpasses the intensity of cutting the aramid fiber paper that fiber makes with high-strength and high-modulus of the present invention and also improves a lot, and better meets customer requirement, asks for an interview following table 2 with specifically contrast situation of common aramid fiber paper.
Table 1: the test result of the high-strength high-modulus fibre of common meta-aramid fibers and present embodiment 1
| Intensity (CN/DTEX) | Modulus | |
| General fibre | ??3.5-4.1 | ??30-50 |
| High-strength high-modulus fibre | ??4.3-4.6 | ??70-90 |
Table 2: the intensity contrast of different aramid fiber paper
The above embodiment only is that preferred implementation of the present invention is described; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (4)
1. the preparation method of a high-strength high-modulus PMIA super-short fiber is characterized in that comprising the steps:
In being the system of organic solvent, amide compound carries out polymerisation in solution with m-phthaloyl chloride and m-phenylene diamine (MPD), obtain comprising the meta-aromatic polyamide solution that mpd-i is a repetitive, carry out the hydrochloric acid that neutralization reaction generates with calcium oxide or calcium hydroxide, get spinning solution, the logarithmic viscosity number that makes spinning solution is at 3-6;
Promptly make the high-strength high-modulus PMIA super-short fiber that length is the 0.5-20 millimeter through wet spinning, cleaning, heat treatment, coiling, cut-out, packing.
2. as the preparation method of claims 1 described high-strength high-modulus PMIA super-short fiber, it is characterized in that described wet spinning is is that the spinning head of the spinneret orifice of 0.01-2 millimeter is extruded with the spinning solution deaeration and by diameter, in temperature is that 20-50 ℃ aqueous coagulation bath forms long filament, and drawing-off doubly makes it have the certain physical mechanical performance through 2-10 in containing calcium chloride water.
3. the preparation method of high-strength high-modulus PMIA super-short fiber as claimed in claim 2 is characterized in that, described heat treatment step is, is to carry out high-temperature shaping under 350-450 ℃ at setting temperature.
4. according to the preparation method of claims 3 described high-strength high-modulus PMIA super-short fibers, it is characterized in that described amide compound is selected from dimethyl formamide or dimethylacetylamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102597783A CN101736431B (en) | 2009-12-24 | 2009-12-24 | Production method of high-strength high-modulus PMIA super-short fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102597783A CN101736431B (en) | 2009-12-24 | 2009-12-24 | Production method of high-strength high-modulus PMIA super-short fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101736431A true CN101736431A (en) | 2010-06-16 |
| CN101736431B CN101736431B (en) | 2012-05-23 |
Family
ID=42460439
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102597783A Active CN101736431B (en) | 2009-12-24 | 2009-12-24 | Production method of high-strength high-modulus PMIA super-short fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101736431B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154726A (en) * | 2011-05-23 | 2011-08-17 | 蓝星（成都）新材料有限公司 | Middle modulus poly (p-phenyl-terephthalamide) fiber and preparation method thereof |
| CN102534839A (en) * | 2010-12-09 | 2012-07-04 | 烟台泰和新材料股份有限公司 | Method for preparing meta-aramid fiber |
| CN102534841A (en) * | 2011-06-08 | 2012-07-04 | 王锡璐 | Poly (p-phenylene terephthalamide) aramid fiber II staple fiber and preparation method thereof |
| CN102605462A (en) * | 2012-02-26 | 2012-07-25 | 昆山华阳复合材料科技有限公司 | High tenacity viscose fiber |
| CN105386136A (en) * | 2015-12-11 | 2016-03-09 | 烟台泰和新材料股份有限公司 | Method for preparing differentiated meta-aramid for filtering tiny dust |
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110144636A (en) * | 2019-06-10 | 2019-08-20 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and preparation method thereof |
| CN110158181A (en) * | 2019-06-21 | 2019-08-23 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber superbhort fiber and preparation method thereof |
| CN112575395A (en) * | 2020-12-04 | 2021-03-30 | 四川辉腾科技股份有限公司 | Heterocyclic aramid fiber solidification forming device and process thereof |
| CN114423892A (en) * | 2019-10-07 | 2022-04-29 | 帝人株式会社 | Method for making fibers comprising meta-aramid |
| CN114481680A (en) * | 2022-03-10 | 2022-05-13 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1265034C (en) * | 2003-04-04 | 2006-07-19 | 东华大学 | Preparation of polyisophthaloyl m-phenylene diamide spinning solution by using semi-continuous twin screw extruder |
-
2009
- 2009-12-24 CN CN2009102597783A patent/CN101736431B/en active Active
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534839A (en) * | 2010-12-09 | 2012-07-04 | 烟台泰和新材料股份有限公司 | Method for preparing meta-aramid fiber |
| CN102154726A (en) * | 2011-05-23 | 2011-08-17 | 蓝星（成都）新材料有限公司 | Middle modulus poly (p-phenyl-terephthalamide) fiber and preparation method thereof |
| CN102154726B (en) * | 2011-05-23 | 2012-11-21 | 蓝星（成都）新材料有限公司 | Middle modulus poly (p-phenyl-terephthalamide) fiber and preparation method thereof |
| CN102534841A (en) * | 2011-06-08 | 2012-07-04 | 王锡璐 | Poly (p-phenylene terephthalamide) aramid fiber II staple fiber and preparation method thereof |
| CN102534841B (en) * | 2011-06-08 | 2014-06-18 | 王锡璐 | Poly (p-phenylene terephthalamide) aramid fiber II staple fiber and preparation method thereof |
| CN102605462A (en) * | 2012-02-26 | 2012-07-25 | 昆山华阳复合材料科技有限公司 | High tenacity viscose fiber |
| CN105386136A (en) * | 2015-12-11 | 2016-03-09 | 烟台泰和新材料股份有限公司 | Method for preparing differentiated meta-aramid for filtering tiny dust |
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110144636A (en) * | 2019-06-10 | 2019-08-20 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and preparation method thereof |
| CN110144636B (en) * | 2019-06-10 | 2021-09-24 | 黄河三角洲京博化工研究院有限公司 | Para-aramid fibrid and preparation method thereof |
| CN110158181A (en) * | 2019-06-21 | 2019-08-23 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber superbhort fiber and preparation method thereof |
| CN114423892A (en) * | 2019-10-07 | 2022-04-29 | 帝人株式会社 | Method for making fibers comprising meta-aramid |
| CN112575395A (en) * | 2020-12-04 | 2021-03-30 | 四川辉腾科技股份有限公司 | Heterocyclic aramid fiber solidification forming device and process thereof |
| CN112575395B (en) * | 2020-12-04 | 2021-09-03 | 四川辉腾科技股份有限公司 | Heterocyclic aramid fiber solidification forming device and process thereof |
| CN114481680A (en) * | 2022-03-10 | 2022-05-13 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same |
| CN114481680B (en) * | 2022-03-10 | 2023-08-22 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material, aerogel and pumping filter membrane material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101736431B (en) | 2012-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101736431B (en) | Production method of high-strength high-modulus PMIA super-short fiber | |
| CN107313126B (en) | Method for producing graphene modified polyamide-6 fiber through high-speed spinning | |
| CN100398707C (en) | Method for preparing meta aromatic polyamide fiber | |
| CN104357939B (en) | A kind of chloride high-performance heterocyclic aramid fiber and its preparation method and application | |
| CN106544748A (en) | A kind of high drawing p-aramid fiber filament industry production method | |
| CN102560716B (en) | Para-aramid chopped fiber with high spinnability and production method thereof | |
| CN103060940B (en) | A kind of preparation method of medium modulus vinal | |
| CN110093679A (en) | A kind of 66/ nylon 6 fiber of graphene modification of nylon and its preparation and application | |
| CN108950716B (en) | Polyamide 56 mowing filament and preparation method thereof | |
| CN109161973A (en) | The production technology of acid fiber by polylactic | |
| CN103806121A (en) | Method for preparing polyisophthaloyl metaphenylene diamine solution without metal ions | |
| KR20090121049A (en) | Aromatic polyamide polymer and method of making the same, and aramid fiber and method of making the same | |
| CN116575138A (en) | Preparation method of bio-based aromatic polyamide fiber | |
| JP5503055B2 (en) | Para-type wholly aromatic copolyamide drawn fiber and method for producing the same | |
| JP2011202327A (en) | Fabric comprising easy-to-dye meta-wholly aromatic polyamide fiber | |
| JP2011026726A (en) | Para type wholly-aromatic copolyamide fiber, and method for producing the same | |
| JP2011017100A (en) | Method for producing carbon fiber | |
| CN111979591B (en) | High-strength high-heat-resistance fine single-fiber nylon 66 fiber and preparation method thereof | |
| CN113668091B (en) | High-strength high-elongation heterocyclic aromatic polyamide fiber and preparation process thereof | |
| CN109468728B (en) | Bamboo fiber fabric | |
| CN113652764A (en) | Surface smooth meta-aramid filament yarn and preparation method thereof | |
| KR20210086467A (en) | Para-aramid staple fiber and manufacturing method of aramid spun yarns application for the high speed carding process | |
| EP4041941A1 (en) | Process for the manufacture of a fiber comprising meta-aramid | |
| CN114921864B (en) | Humidity response guar gum fiber and preparation method thereof | |
| CN103476976A (en) | Method for manufacturing polyethylene terephthalate drawn fiber, polyethylene terephthalate drawn fiber, and tire cord |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: YANTAI TAYHO ADVANCED MATERIALS CO., LTD. Free format text: FORMER OWNER: YANTAI SPANDEX CO., LTD. Effective date: 20111231 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Song Xiquan Inventor after: Sun Maojian Inventor after: Song Cuiyan Inventor after: Wang Yinchao Inventor after: Zhang Chunhua Inventor before: Song Cuiyan Inventor before: Song Xiquan Inventor before: Wang Yinchao Inventor before: Wang Xue Inventor before: Gao Dong |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: SONG CUIYAN SONG XIQUAN WANG YINCHAO WANG XUE GAO DONG TO: SONG XIQUAN SUN MAOJIAN SONG CUIYAN WANG YINCHAO ZHANG CHUNHUA |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20111231 Address after: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Applicant after: YANTAI TAYHO ADVANCED MATERIALS Co.,Ltd. Address before: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Applicant before: YANTAI SPANDEX Co.,Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Patentee after: Taihe New Material Group Co.,Ltd. Address before: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Patentee before: YANTAI TAYHO ADVANCED MATERIALS Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |