CN102154727A - High-intensity poly(terephthaloyl-p-phenylene diamine) (PPTA) fiber and preparation method thereof - Google Patents
High-intensity poly(terephthaloyl-p-phenylene diamine) (PPTA) fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-intensity poly(terephthaloyl-p-phenylene diamine) (PPTA) fiber. The fiber is prepared by performing special treatment on a PPTA polymer, which has the logarithmic viscosity of 5.5-8.0 dL/g and serves as a raw material, in the dry-jet wet spinning process. The specific indexes of the PPTA fiber are that: the bundle fineness is 300-3,000 D, the intensity is 24-30 g/D, the elongation percentage is 3.6-4.2 percent, the modulus is 350-650 g/D, the water content is 4-10 percent, and the logarithmic viscosity is 5.0-7.5 dL/g. In the dry-jet wet spinning process, the spinning speed is controlled at 100-500 m/min, and the diameter of a spinning hole is less than or equal to 0.05 millimeter, so that a PPTA fiber product with ultrahigh intensity and elongation percentage is obtained. The product has high impact resistance and bullet resistance, and is relatively suitable for military bullet resistance; and the blank in corresponding aspect in China is filled up.
Description
Technical field
The present invention relates to the artificial fibre field; particularly a kind of PPTA with logarithm viscosity 5.5-8.0dL/g (PPTA) polymer is a raw material; by the special treatment in the spinning process of dry-jet wet-spinning, a kind of high strength Fanglun 1414 who is applicable to industrial scale production of acquisition and preparation method thereof.
Background technology
PPTA (PPTA) fiber adopts the cryogenic fluid polycondensation reaction synthetic in nineteen sixty-five by du pont company, utilizes PPTA/H then
2SO
4Solution has liquid crystal behavior, has invented the method for dry-jet wet-spinning, thereby obtains high-performance Fanglun 1414 (being called for short " aramid fiber II ").The patent of correlation technique is delivered in the U.S. successively at 1970-1985, for example the patent No.: 3671542,3819587,19730361818,3767756,3869429,3849430,4726922,5001219,5009830,19760720849,19880182826,1980012088,19970950250 etc.
Du pont company carries out the PPTA fiber production since the developing target market of small lot in 1972, and nineteen eighty-two begins to carry out suitability for industrialized production, and name of product is Kevlar.Dutch Akzo dropped into the production of PPTA aramid fiber in 1985, and name of product is Twaron.Japan Supreme Being people company merged the Twaron business of Dutch Akzo company in 2005, and continued to expand output and compete with E.I.Du Pont Company.Also at test manufacture PPTA and pulp in 1985, this productions stopped in from 1990 to 2000 substantially in Korea S Ke Long company, in recovery development in 2006 and found the factory.
Aramid fiber II fiber product has multiple commercial variety, and comprehensive international market commodity can roughly be divided into following a few class: 1. general aramid fiber II fiber.Its long yarn intensity is in the 22-23g/d scope, percentage elongation 3.5-3.6%, and the about 550g/d of modulus, this product is used for Application Areass such as tire cord, reinforcing rubber mostly.2. modulus product in the aramid fiber II.Its long yarn intensity is about 23.7g/d, and the about 750g/d of modulus, this product mostly are used for Application Areass such as optical cable reinforcement, unidirectional composite material reinforcement.3. aramid fiber II high modulus product.The about 22-23g/d of its long yarn intensity, modulus 800-950g/d is used for the composite reinforcement mostly.4. also have high strength aramid fiber II fiber product on the market in recent years, the about 26.5-27.5g/d of its long yarn intensity is used for shellproof military use more.In raising variety, some high strength kind restricts export and is supplied to China.
The polymerisation of preparation PPTA is shown below:
The main physical and chemical performance of PPTA comprise strand-NH or-CO end group, molecular weight, molecular weight distribution, density, moisture content, vitrification point, softening temperature, decomposition temperature, inorganic salt content, ash etc., wherein molecular weight and molecular weight distribution having the greatest impact to fibre property.But survey because molecular weight and molecular weight distribution are very difficult, therefore, use logarithm viscosity more to help grasping fast the correlation technique information of PPTA and fiber thereof, fully reflect the technological approaches and the technological level of polymerization and spinning as technical indicator.
The molecular weight of directly measuring PPTA is difficulty very, but available its dilution heat of sulfuric acid viscosity is done indication indirectly, and general " logarithm viscosity " (the inherent viscosity) that adopt is defined as follows:
η in the formula
InhBe logarithm viscosity, η
RelBe relative viscosity, i.e. the ratio of the viscosity of polymer solution and solvent viscosity, C is the polymer concentration of solution.The mensuration of the logarithm concentration of PPTA is in the 96-98% concentrated acid, and getting C is 0.5g/dL, is to record under 30 ℃ in temperature.The logarithm viscosity number of PPTA alters a great deal in the scope of 1 ~ 10dL/g in the document.
Polymer molecular weight influences the performance of its derivative, and high molecular weight polymers is all adopted in general plastic cement and synthetic fiber industry as far as possible.Make the PPTA fiber too, molecular weight influences the performance of fiber, especially physical property, for example fibre strength and modulus.But the technology of making fiber when molecular weight is too high is very difficult, influences industrial efficiency.
The fusing point of PPTA can not be melt-spun into fiber on its heat decomposition temperature (about 550 ℃).By the technology of generally acknowledging in the industry, PPTA dissolves in the concentrated sulfuric acid, its concentration is when 12-19.6%, can form a liquid crystal aligning solution (Anisctropic Solution), this solution (also claiming " spinning slurry "), dry-jet wet-spinning (dry-jet wet spinning) method by generally acknowledging can make high-performance fiber.Dry-jet wet-spinning still belongs to a kind of wet spinning process of synthetic fiber, is characterized in: spinnerets is positioned at the coagulating bath top during spinning, and solidifies the air layer gap that has certain altitude between the liquid level.Spin slurry down,, enter coagulating bath, derive from solidifying pipe through air layer by the spinnerets spray.The slurry silk is solidified the liquid extraction when entering coagulating bath, precipitate into silk, and most of sulfuric acid diffuses into solidification liquid.Solidify the spun filament that obtains and after technologies such as washing, neutralization, washing, drying, be wound into fiber product.
The applicant is in " a kind of poly P phenylene diamine terephthalamide fiber and preparation method thereof " (application number 200910216761.X) of application on December 14th, 2009, wherein disclosed this poly P phenylene diamine terephthalamide fiber specific targets comprise: the bundle yarn fiber number 300-3000 dawn, the intensity 18-26 gram/dawn, percentage elongation 3.2-3.8%, modulus is the 350-650 gram/dawn, moisture content 3-10%, logarithm viscosity 4.0-7.5dL/g.
Summary of the invention
The purpose of this invention is to provide a kind of PPTA with logarithm viscosity 5.5-8.0dL/g (PPTA) polymer is raw material; by the special treatment in the spinning process of dry-jet wet-spinning, a kind of high strength Fanglun 1414 who is applicable to industrial scale production of acquisition and preparation method thereof.This poly P phenylene diamine terephthalamide fiber has good impact resistance and ballistic performance, relatively is applicable to military shellproof aspect, has filled up domestic blank.
Concrete technical scheme of the present invention is as follows:
A kind of high strength PPTA (PPTA) fiber, it is characterized in that: PPTA (PPTA) polymer with logarithm viscosity 5.5-8.0dL/g is a raw material, and be prepared from by the special treatment in the spinning process of dry-jet wet-spinning, this Fanglun 1414's specific targets comprise: the bundle yarn fiber number 300-3000 dawn, the intensity 24-30 gram/dawn, percentage elongation 3.6-4.2%, the modulus 350-650 gram/dawn, moisture content 4-10%, logarithm viscosity 5.0-7.5dL/g.
The preferred 6.0-7.5dL/g of logarithm viscosity of described high strength PPTA (PPTA) polymer raw material.
Described high strength Fanglun 1414's preparation method, synthetic and the dry-jet wet-spinning step that comprises PPTA (PPTA) polymer raw material, it is characterized in that: in the spinning process of dry-jet wet-spinning, spinning speed is controlled at 100-500m/min, spinneret orifice diameter≤0.05mm.
The concrete steps that employing cryogenic fluid polycondensation method of the present invention prepares PPTA (PPTA) polymer are as follows:
The preparation of A, raw material
P-phenylenediamine (PPD) (p-phenylene diamine) [PPD],
To benzene two tetramethyl acyl chlorides (Terephthaloyl chloride) [TPC],
Helping polysalt is cosolvent: calcium chloride [CaCl
2];
Wherein: the mol ratio of PPD/TPC equals 1.0-1.015, CaCl
2The mol ratio of/PPD equals 1.2-1.7, and the solid content of polyblend is 9-12%;
The polymerization of B, raw material
Reactor with after the nitrogen feeding oven dry adds dry NMP/CaCl then
2Solvent and dry highly purified p-phenylenediamine (PPD) (PPD), rotating mixer, after mixing, with the chilled water chuck of reactor, the mixture of p-phenylenediamine (PPD) PPD and solvent NMP is dissolved gradually, and in 1 minute to 24 hours, be cooled to 0-20 ℃, the paraphthaloyl chloride (TPC) that adds 20-40% wt again, continue to stir the temperature control cooling, after abundant reaction in 1 minute to 24 hours to 0-20 ℃, again in the paraphthaloyl chloride TPC of 1 minute to 24 hours adding surplus; In this process the chuck chilled water is changed to 20-40 ℃ of warm water, reaction temperature is increased to 10-20 ℃ gradually, and through after stirring, temperature is gradually steady, rises to 20-50 ℃ naturally; After finishing to reaction, reactant mixture autoreaction still being taken out, is the NaOH solution neutralization of 10-20% with percentage by weight earlier, spends deionised water 10-40 time again, drying then, the PPTA polymer that can obtain having 5.5-8.0dL/g logarithm viscosity.
Shown in dry-jet wet spinning process comprise solidify, extraction, spinning, washing, neutralization, drying, oil, operation such as coiling.
The concrete steps of described spinning are as follows:
With above-mentioned logarithm viscosity 5.5-8.0dL/g PPTA (PPTA) polymer, adding concentration is in the sulfuric acid of 98-100%, through strong agitation and be warming up to 78-82 ℃, making concentration is the slurry that spins of 19.4-19.5%, and slurries are sprayed from spinnerets by gear pump metering back after filtering; Spinnerets has more than 100 and spins the hole, its aperture≤0.05mm, after spinning slurry ejection and spinning the hole is the pulping silk, pass through the 6-8mm air layer, enter the solution face that solidifies, pass through the pipe that solidifies at coagulating basin center then, outflow below managing, coagulation bath temperature 0-10 ℃, the acid content of solidification liquid is less than 15%, and coagulating basin solidifies pipe with funnel type or cast or injecting type; Contained sulfuric acid is partly extracted in the slurry silk at this moment, becomes vitriolated wet yarn; Wet yarn continues dirty, turns in short distance, removes most of acid solution; The wet yarn of gained on multistage rotating cylinder roller, carry out the order for the washing of washing/alkali cleaning/washing/washing, in and technology, use drum dryer 120-140 ℃ of drying then.In washing, neutralization and drying process, it is stable to keep yarn speed, avoid wet yarn to stretch and surpass 0.5%, dried yarn oil the back with the up-coiler rolling on paper web, winding speed is 100 ~ 500m/min.
Good effect of the present invention is as follows:
1, industrial cost is low, the efficient height.
In the prior art, it is extremely important to the selection of polymer logarithm viscosity that the high modulus fibre product is made in industrialization.The polymer of employing hyperviscosity carries out slurrying and spinning operation is all very difficult, for example logarithm viscosity is more than 8.0dl/g, its polymerization time is longer more than 2 times at the normal polymerization time below the 8.0dl/g than logarithm viscosity, and it is all very difficult to join slurry and spinning operation.Owing to the slurry viscosity height, required stirring and dissolution time are very long when joining slurry; Can be owing to spin slurry pressure superelevation when spinning, cause measuring pump, filament spinning component easily and spin the leakage or the damage of plate; And spinning efficiency is very low, significantly increases running cost, is unwell to suitability for industrialized production.And adopt low viscous polymer, and be that 4.0-5.5dL/g carries out spinning as logarithm viscosity, though easy to operate, the properties of product of gained fiber do not reach requirement, especially intensity and modulus are very low.It is the polymer of 5.5-8.0dl/g that the present invention adopts logarithm viscosity, asks it moderate, avoids polymerization on the one hand, joins the difficulty in slurry and the spinning operation, guarantees that the gained fiber has excellent properties on the one hand, the process efficiency height, and the industrialization cost is low.
2, the present invention is in the spinning process of dry-jet wet-spinning, and by spinning speed is controlled at 100-500m/min, spinneret orifice diameter selection≤0.05mm has obtained to have the poly P phenylene diamine terephthalamide fiber product of Extra High Strength and percentage elongation.This product has good impact resistance and ballistic performance, relatively is applicable to military shellproof aspect, has filled up domestic blank.
The typical physical performance of this product and similar aramid fiber II product more as shown in table 1:
This product of table 1 compares with the typical physical performance of similar aramid fiber II product
The specific embodiment
Embodiment 1
The manufacture method of a kind of high strength PPTA (PPTA) fiber, it is characterized in that: PPTA (PPTA) polymer with logarithm viscosity 6.5dL/g is a raw material, and be prepared from by the special treatment in the spinning process of dry-jet wet-spinning, this Fanglun 1414's specific targets comprise: bundle yarn 1500 dawn of fiber number, 25 gram/the dawn of intensity, percentage elongation 4.0%, 475 gram/dawn of modulus, moisture content 5%, logarithm viscosity 6.2dL/g.
Described high strength Fanglun 1414's preparation method, synthetic and the dry-jet wet-spinning step that comprises PPTA (PPTA) polymer raw material, it is characterized in that: in the spinning process of dry-jet wet-spinning, spinning speed is controlled at 300m/min, spinneret orifice diameter 0.05mm.
The concrete steps that described employing cryogenic fluid polycondensation method prepares PPTA (PPTA) polymer are as follows:
The preparation of A, raw material
P-phenylenediamine (PPD) (p-phenylene diamine) [PPD],
To benzene two tetramethyl acyl chlorides (Terephthaloyl chloride) [TPC],
Helping polysalt is cosolvent: calcium chloride [CaCl
2];
Wherein: the mol ratio of PPD/TPC equals 1.0, CaCl
2The mol ratio of/PPD equals 1.4, and the solid content of polyblend is 11%;
The polymerization of B, raw material
Reactor with after the nitrogen feeding oven dry adds dry NMP/CaCl then
2Solvent and dry highly purified p-phenylenediamine (PPD) (PPD), rotating mixer, after mixing, enable the chilled water chuck of reactor, the mixture of p-phenylenediamine (PPD) PPDA and solvent NMP is dissolved gradually and in 2 hours, be cooled to 20 ℃, add total amount 30% paraphthaloyl chloride (TPC) again, continue to stir cooling, after abundant reaction in 24 hours to 0 ℃, add the paraphthaloyl chloride TPC of surplus again; In this process the chuck chilled water is changed to 20 ℃ of warm water, reaction temperature is increased to 10 ℃ gradually, and through after stirring, temperature is gradually steady, rises to 30 ℃ naturally; After finishing to reaction, reactant mixture autoreaction still being taken out, is earlier 15% NaOH solution neutralization with percentage by weight, spends deionised water again 14 times, drying then, the PPTA polymer that can obtain having 6.5dL/g logarithm viscosity;
Shown in dry-jet wet spinning process comprise solidify, extraction, spinning, washing, neutralization, drying, oil, operation such as coiling.
With above-mentioned logarithm viscosity 6.5dL/g PPTA (PPTA) polymer, add concentration and be in 99.6% the sulfuric acid, through strong agitation and be warming up to 80 ℃, make concentration and be 19.4% the slurry that spins, slurries are sprayed from spinnerets by gear pump metering back after filtering; Spinnerets has more than 100 and spins the hole, and its aperture is 0.05mm.After spinning slurry ejection and spinning the hole is the pulping silk, through the 7mm air layer, enters the solution face that solidifies, then through the pipe that solidifies at coagulating basin center, and outflow below managing, coagulation bath temperature 0-10 ℃, the acid content of solidification liquid is 8%, coagulating basin solidifies pipe with cast; Contained sulfuric acid is partly extracted in the slurry silk at this moment, becomes vitriolated wet yarn; Wet yarn continues dirty, turns in short distance, removes most of acid solution; The wet yarn of gained on multistage rotating cylinder roller, carry out order for the washing of washing/alkali cleaning/washing/alkali cleaning/washing, in and technology, use drum dryer 130 ℃ of dryings then, dried yarn oils, and afterwards the rolling of usefulness up-coiler is on paper web, winding speed is 300m/min
The long yarn performance of gained sees table 2 for details.
The mechanical property of table 2 fiber
Claims (7)
1. high strength Fanglun 1414, it is characterized in that: the PPTA polymer with logarithm viscosity 5.5-8.0dL/g is a raw material, and be prepared from by the special treatment in the spinning process of dry-jet wet-spinning, this Fanglun 1414's specific targets comprise: the bundle yarn fiber number 300-3000 dawn, the intensity 24-30 gram/dawn, percentage elongation 3.6-4.2%, modulus 350-650 gram/dawn, moisture content 4-10%, logarithm viscosity 5.0-7.5dL/g.
2. the high strength Fanglun 1414 is poly-according to claim 1, and it is characterized in that: the logarithm viscosity of described high strength PPTA polymer raw material is 6.0-7.5dL/g.
3. preparation method of high strength Fanglun 1414 as claimed in claim 1 or 2, synthetic and the dry-jet wet-spinning step that comprises the PPTA polymer raw material, it is characterized in that: in the spinning process of dry-jet wet-spinning, spinning speed is controlled at 100-500m/min, spinneret orifice diameter≤0.05mm.
4. as the preparation method of high strength Fanglun 1414 as described in the claim 3, it is characterized in that: the synthetic employing cryogenic fluid polycondensation method of described PPTA polymer raw material, concrete steps are as follows:
The preparation of A, raw material
P-phenylenediamine (PPD) (p-phenylene diamine) [PPD],
To benzene two tetramethyl acyl chlorides (Terephthaloyl chloride) [TPC],
Helping polysalt is cosolvent: calcium chloride [CaCl
2];
Wherein: the mol ratio of PPD/TPC equals 1.0-1.015, CaCl
2The mol ratio of/PPD equals 1.2-1.7, and the solid content of polyblend is 9-12%;
The polymerization of B, raw material
Reactor with after the nitrogen feeding oven dry adds dry NMP/CaCl then
2Solvent and dry highly purified p-phenylenediamine (PPD), rotating mixer, after mixing, enable the chilled water chuck of reactor, the mixture of p-phenylenediamine (PPD) PPD and solvent NMP is dissolved gradually and in 1 minute to 24 hours, be cooled to 0-20 ℃, add the paraphthaloyl chloride of the 20-40% wt of total amount again, continue to stir temperature control, through abundant reaction back in 1 minute to 24 hours to 0-20 ℃, again in 1 minute in 24 hours the paraphthaloyl chloride TPC of adding surplus; In this process the chuck chilled water is changed to 20-40 ℃ of warm water, reaction temperature is increased to 10-20 ℃ gradually, and through after stirring, temperature is gradually steady, rises to 20-50 ℃ naturally; After finishing to reaction, reactant mixture autoreaction still being taken out, is the NaOH solution neutralization of 10-20% with percentage by weight earlier, spends deionised water 10-40 time again, drying then, the PPTA polymer that can obtain having 5.5-8.0dL/g logarithm viscosity.
5. as the preparation method of high strength Fanglun 1414 as described in the claim 3, it is characterized in that: described dry-jet wet spinning process comprise solidify, extraction, spinning, washing, neutralization, drying, operation oils, reels.
6. as the preparation method of high strength Fanglun 1414 as described in the claim 3, it is characterized in that: the concrete steps of described spinning are as follows:
With above-mentioned logarithm viscosity 5.5-8.0dL/g PPTA polymer, adding concentration is in the sulfuric acid of 98-100%, through strong agitation and be warming up to 78-82 ℃, making concentration is the slurry that spins of 19.4-19.5%, and slurries are sprayed from spinnerets by gear pump metering back after filtering; Spinnerets has 100-2000 to spin the hole, its aperture is≤0.05mm, after spinning slurry ejection and spinning the hole is the pulping silk, pass through the 6-8mm air layer, enter the solution face that solidifies, pass through the pipe that solidifies at coagulating basin center then, outflow below managing, coagulation bath temperature 0-10 ℃, the acid content of solidification liquid is less than 15%, and coagulating basin solidifies pipe with funnel type or cast; Contained sulfuric acid is partly extracted in the slurry silk at this moment, becomes vitriolated wet yarn; Wet yarn continues dirty, turns in short distance, removes most of acid solution; The wet yarn of gained on multistage rotating cylinder roller, carry out the order for the washing of washing/alkali cleaning/washing/washing, in and technology, use drum dryer 120-140 ℃ of drying then.
7. in washing, neutralization and drying process, it is stable to keep yarn speed, avoid wet yarn to stretch and surpass 0.5%, dried yarn oil the back with the up-coiler rolling on paper web, winding speed is 100-500m/min.
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| CN103572390A (en) * | 2013-10-21 | 2014-02-12 | 中蓝晨光化工研究设计院有限公司 | Dry spraying-wet spinning method for manufacturing aramid III fiber |
| CN104404644A (en) * | 2014-11-20 | 2015-03-11 | 东华大学 | Method for preparing spinning pulp through dissolution of PPTA resin with solid foamed sulfuric acid |
| CN104451935A (en) * | 2014-12-12 | 2015-03-25 | 东华大学 | Solidification method for preparing para-aramid by adopting dry jet-wet spinning |
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| CN107629206A (en) * | 2017-10-17 | 2018-01-26 | 蓝星（成都）新材料有限公司 | A kind of preparation method of Fanglun l414 fiber |
| CN109487354A (en) * | 2018-11-07 | 2019-03-19 | 东华大学 | A kind of method that one-step method prepares high-modulus p-aramid fiber |
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| CN114351276A (en) * | 2021-12-23 | 2022-04-15 | 烟台泰和新材料股份有限公司 | High-strength para-aramid fiber and preparation method thereof |
| CN118440316A (en) * | 2024-05-10 | 2024-08-06 | 江苏盛邦新材股份有限公司 | Preparation method of spinning-grade poly (p-phenylene terephthamide) polymer and fiber thereof |
| CN118440316B (en) * | 2024-05-10 | 2024-11-08 | 江苏盛邦新材股份有限公司 | Preparation method of spinning-grade poly (p-phenylene terephthamide) polymer and fiber thereof |
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Application publication date: 20110817 |