CN104404645B - A kind of method that aramid fiber spinning slurry directly prepared by PPTA resin - Google Patents
A kind of method that aramid fiber spinning slurry directly prepared by PPTA resin Download PDFInfo
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- CN104404645B CN104404645B CN201410728119.0A CN201410728119A CN104404645B CN 104404645 B CN104404645 B CN 104404645B CN 201410728119 A CN201410728119 A CN 201410728119A CN 104404645 B CN104404645 B CN 104404645B
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Abstract
The present invention relates to a kind of method that aramid fiber spinning slurry directly prepared by PPTA resin, directly wash with water after neutralized for the PPTA resin synthesized, then PPTA resin is dehydrated, the PPTA resin after being dehydrated；By the PPTA resin cooling after dehydration, under stirring condition, it is passed through SO3Gas, keeping system temperature is 11～13 DEG C, obtains concentrated sulphuric acid, then heats to 80 90 DEG C and carry out dissolving and pre-deaeration, obtain liquid crystal solution, deaeration, to obtain final product.The inventive method good mixing effect, dissolved efficiency is high, is greatly shortened the preparation time from resin to spinning slurry, and in course of dissolution, the degraded of resin is fewer.
Description
Technical field
The invention belongs to the preparation field of spinning slurry, directly prepare aramid fiber spinning slurry particularly to a kind of PPTA resin
Method.
Background technology
PPTA (PPTA) fiber is a kind of high-performance fiber being widely used in every field.It by
The liquid crystal solution of PPTA resin/concentrated sulphuric acid is prepared by dry-jet wet-spinning.At present, the spinning of industrial PPTA resin/concentrated sulphuric acid
The resin being fully dried mainly directly is mixed with concentrated sulphuric acid, shears by the preparation method of silk serosity, rising temperature for dissolving.Also have specially
PPTA resin is first mixed by profit report with freezing concentrated sulphuric acid, and then heat up shearing, forms liquid crystal serosity.Traditional is spun
For silk serosity preparation method, resin contacts that rear surface is the most swelling, heating inter-adhesive thus serious knot occur
Group's phenomenon, causes the resin being coated in agglomerate to be difficult to adsorb further sulphuric acid, thus is difficult to further mix homogeneously and dissolving,
Hinder being smoothed out of dissolving, need to coordinate the shear action of strength to complete in being blended in the long time to dissolve.
Owing to the acidity of sulphuric acid is very strong, long dissolving can cause the violent degraded of resin.Resin is mixed with freezing concentrated sulphuric acid
For conjunction method, the mode of solid-solid blend advantageously reduces the harm of resin conglomeration, improves the uniformity of serosity.But due to
Resinous powder particles is less, and proportion is less than sulphuric acid granule, and the mixture form therefore formed is that sulphuric acid particle surface has adsorbed very
Many resin particles, are equivalent to sulphuric acid and are dispersed in resin, still there will be a certain degree of clustering phenomena.And need
Concentrated sulphuric acid is freezing, and the time of consuming is longer, and resin degraded is big, and energy consumption is the biggest, is unfavorable for improving production efficiency.
Summary of the invention
The technical problem to be solved is to provide a kind of method that aramid fiber spinning slurry directly prepared by PPTA resin, this
Invention use the PPTA resin that is not completely dried as raw material, its loose structure be conducive to sulphuric acid to the infiltration within resin,
Accelerate the dissolving of resin, be simultaneously also beneficial to improve the uniformity of serosity and prevent the violent degraded of PPTA.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin of the present invention, including:
(1) directly washing with water after neutralized for the PPTA resin containing a large amount of micropores synthesized, be swapped out in resin is molten
Agent and salinity, be then dehydrated PPTA resin, but moisture not exclusively remove, the PPTA after being dehydrated
Resin；Wherein in the PPTA resin after dehydration, the mass ratio of water and resin is 1:1.0～1:1.6；
(2) by the PPTA resin cooling after dehydration, under stirring condition, it is passed through SO3Gas, keeping system temperature is 11～13 DEG C,
Gas is made gradually to be only absorbed by the water formation concentrated sulphuric acid, SO3After GAS ABSORPTION terminates, then heat to 80-90 DEG C and carry out molten
Solve and pre-deaeration, obtain liquid crystal solution, deaeration, obtain aramid fiber spinning slurry.
The logarithmic viscosity number of the PPTA resin synthesized in described step (1) is 4.0-8.0dl/g.
Described step is cooled to 0-2 DEG C in (2).
Described step (2) is passed through the SO of 5～10MPa3Gas；The time of being passed through is 0.1-1h.
Described step is passed through SO in (2) under agitation3Gas；Wherein, the resin of humidity first it is passed through with slower speed
In (resin after dehydration), the beneficially heat radiation of system, when water absorb SO3The sulfuric acid concentration produced after gas reaches 80%
After, heat release reduces, and that can accelerate gas is passed through speed.
In described step (2), the concentration of concentrated sulphuric acid is 99.8～100.2%.
In described step (2), the mass percentage concentration of aramid fiber spinning slurry is 15.5～23%.
Described step (2) is dissolved and pre-deaeration 0.2-0.8h altogether.
The present invention is directly to washing the SO being passed through high pressure in later half dried resin3Gas, the water in resin micropore absorbs SO3Raw
Become concentrated sulphuric acid, then carry out rising temperature for dissolving, save the time that resin is dried and mixes.It is also an advantage of the present invention that, just close
The resin become is the structure of a kind of multiple hole, in solvent during water has displaced hole in cleaning process access aperture hole, therefore
SO is absorbed at water3After generating concentrated sulphuric acid, resin has reached the effect mixed homogeneously with concentrated sulphuric acid.
Beneficial effect
The present invention uses the PPTA resin not being completely dried as raw material, and its loose structure is conducive to sulphuric acid within resin
Infiltration, accelerates the dissolving of resin, is simultaneously also beneficial to improve the uniformity of serosity and prevent the violent degraded of PPTA；
The inventive method good mixing effect, dissolved efficiency is high, is greatly shortened the preparation time from resin to spinning slurry, and
In course of dissolution, the degraded of resin is fewer.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
By 100 kilograms of logarithmic viscosity numbers cleaning through water be 6.0dl/g, the PPTA that mass ratio is 1:1.2 of water and resin
Resin adds multiaxis planetary stirrer and is stirred, and wherein, is passed through freezing liquid in the chuck of planetary stirrer, by humidity tree
The temperature of fat controls at about 1 DEG C.
The SO of 5MPa it is slowly introducing in wet resin3Gas, keeps system temperature at 11 DEG C.After 0.8h, in resin
Water absorbs SO3Concentration reaches 80%, by SO3The amount of gas increases, and after 10min, the concentration of sulphuric acid reaches 99.8%.
Mixture is warming up to 85 DEG C carry out dissolving and pre-deaeration, after 0.5h, obtains the liquid of the PPTA/ sulphuric acid that concentration is 18.1%
Brilliant solution.
Embodiment 2
By 100 kilograms of logarithmic viscosity numbers cleaning through water be 5.8dl/g, the PPTA that mass ratio is 1:1.6 of water and resin
Resin adds multiaxis planetary stirrer and is stirred, and wherein, is passed through freezing liquid in the chuck of planetary stirrer, by humidity tree
The temperature of fat controls at about 1 DEG C.
The SO of 5MPa it is slowly introducing in wet resin3Gas, keeps system temperature at 11 DEG C.After 0.6h, in resin
Water absorbs SO3Concentration reaches 80%, by SO3The amount of gas increases, and after 10min, the concentration of sulphuric acid reaches 99.9%.
Mixture is warming up to 85 DEG C carry out dissolving and pre-deaeration, obtains the liquid crystal solution of PPTA/ sulphuric acid after 0.4h, will obtain
Liquid crystal solution pump into rear road and carry out deaeration, obtaining the concentration that uniform concentration is 22.7% is PPTA/ sulfuric acid spin serosity.
Embodiment 3
By 100 kilograms of logarithmic viscosity numbers cleaning through water be 7.8dl/g, the PPTA that mass ratio is 1:1.1 of water and resin
Resin adds multiaxis planetary stirrer and is stirred, and wherein, is passed through freezing liquid in the chuck of planetary stirrer, by humidity tree
The temperature of fat controls at about 1 DEG C.
The SO of 10MPa it is slowly introducing in wet resin3Gas, keeps system temperature at 13 DEG C.After 0.5h, in resin
Water absorb SO3Concentration reaches 80%, by SO3The amount of gas increases, and after 10min, the concentration of sulphuric acid reaches 100.1%.
Mixture is warming up to 85 DEG C carry out dissolving and pre-deaeration, obtains the liquid crystal solution of PPTA/ sulphuric acid after 0.5h, will obtain
Liquid crystal solution pump into rear road and carry out deaeration, obtain the PPTA/ sulfuric acid spin serosity that uniform and stable concentration is 16.8%.
Claims (7)
1. the method that aramid fiber spinning slurry directly prepared by PPTA resin, including:
(1) directly wash with water after neutralized for the PPTA resin synthesized, then PPTA resin is dehydrated, is taken off
PPTA resin after water；Wherein in the PPTA resin after dehydration, the mass ratio of water and resin is 1:1.0～1:1.6；
(2) by the PPTA resin cooling after dehydration, under stirring condition, it is passed through SO3Gas, keeping system temperature is 11～13 DEG C,
Obtain concentrated sulphuric acid, then heat to 80-90 DEG C and carry out dissolving and pre-deaeration, obtain liquid crystal solution, deaeration, obtain aramid fiber
Spinning slurry.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
The logarithmic viscosity number of the PPTA resin being directly synthesized out in step (1) is 4.0-8.0dl/g.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
Step is cooled to 0-2 DEG C in (2).
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
Step (2) is passed through the SO of 5～10MPa3Gas；The time of being passed through is 0.1-1h.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
In step (2), the concentration of concentrated sulphuric acid is 99.8～100.2%.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
In step (2), the mass percentage concentration of aramid fiber spinning slurry is 15.5～23%.
The method that aramid fiber spinning slurry directly prepared by a kind of PPTA resin the most according to claim 1, it is characterised in that: described
Step (2) is dissolved and pre-deaeration 0.2-0.8h altogether.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410728119.0A CN104404645B (en) | 2014-12-03 | 2014-12-03 | A kind of method that aramid fiber spinning slurry directly prepared by PPTA resin |
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| CN201410728119.0A CN104404645B (en) | 2014-12-03 | 2014-12-03 | A kind of method that aramid fiber spinning slurry directly prepared by PPTA resin |
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| CN104404645B true CN104404645B (en) | 2016-08-17 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115522285B (en) * | 2022-09-19 | 2023-10-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of aromatic polyamide aerogel fiber |
| CN115928230A (en) * | 2022-12-05 | 2023-04-07 | 安徽元琛环保科技股份有限公司 | Device and method for preparing aramid fiber precursor through dry-jet wet spinning |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4148774A (en) * | 1978-04-07 | 1979-04-10 | Monsanto Company | Process for preparing anisotropic oleum dopes of polyamides by polymerizing in sulfur trioxide |
| EP2053147A1 (en) * | 2007-10-23 | 2009-04-29 | Teijin Aramid B.V. | Method for spinning and washing aramid fiber and recovering sulfuric acid |
| CN101476173A (en) * | 2009-01-20 | 2009-07-08 | 赵海鹏 | Direct spinning process for preparing PPTA fibre by end capping resin method |
| CN202072533U (en) * | 2011-05-31 | 2011-12-14 | 上海舟汉纤维材料科技有限公司 | Continuous treatment device for sulfuric acid waste water |
| CN103014881A (en) * | 2012-12-31 | 2013-04-03 | 东华大学 | Device and method for controlling molecular weight degradation in PPTA (Poly-p-phenyleneterephthamide) resin dissolving process |
| CN103910891A (en) * | 2014-03-13 | 2014-07-09 | 中科院广州化学有限公司南雄材料生产基地 | Dissolving method of para-aramid and applications of the method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5653207A (en) * | 1979-10-02 | 1981-05-12 | Teijin Ltd | Production of aromatic polyamide fiber |
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2014
- 2014-12-03 CN CN201410728119.0A patent/CN104404645B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4148774A (en) * | 1978-04-07 | 1979-04-10 | Monsanto Company | Process for preparing anisotropic oleum dopes of polyamides by polymerizing in sulfur trioxide |
| EP2053147A1 (en) * | 2007-10-23 | 2009-04-29 | Teijin Aramid B.V. | Method for spinning and washing aramid fiber and recovering sulfuric acid |
| CN101476173A (en) * | 2009-01-20 | 2009-07-08 | 赵海鹏 | Direct spinning process for preparing PPTA fibre by end capping resin method |
| CN202072533U (en) * | 2011-05-31 | 2011-12-14 | 上海舟汉纤维材料科技有限公司 | Continuous treatment device for sulfuric acid waste water |
| CN103014881A (en) * | 2012-12-31 | 2013-04-03 | 东华大学 | Device and method for controlling molecular weight degradation in PPTA (Poly-p-phenyleneterephthamide) resin dissolving process |
| CN103910891A (en) * | 2014-03-13 | 2014-07-09 | 中科院广州化学有限公司南雄材料生产基地 | Dissolving method of para-aramid and applications of the method |
Non-Patent Citations (1)
| Title |
|---|
| PPTA低温硫酸溶解工艺研究;杨拯等;《高科技纤维与应用》;20100430;第35卷(第02期);第6-9页 * |
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