CN205517338U - P phenylenediamine's continuous dissolving device - Google Patents
P phenylenediamine's continuous dissolving device Download PDFInfo
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- CN205517338U CN205517338U CN201620323856.7U CN201620323856U CN205517338U CN 205517338 U CN205517338 U CN 205517338U CN 201620323856 U CN201620323856 U CN 201620323856U CN 205517338 U CN205517338 U CN 205517338U
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Abstract
The utility model belongs to a polymer synthesis technology field relates to a P phenylenediamine's continuous dissolving device, and in particular to counterpoint is resin continuous polymerization in -process monomer P phenylenediamine's continuous dissolving device for the aramid fiber, and the device has realized that PPD dissolves the intermittent type formula that replaces using always in succession and dissolves to it all is continuous operation to make all processes of PPTA polymeric, and then has not only guaranteed the stability of resin molecular weight, has realized the uniformity of resin color and luster moreover.
Description
Technical field
This utility model belongs to macromolecule synthesising technology field, relates to the continuous-dissolution device of a kind of p-phenylenediamine, particularly to one
Para-aramid fiber continuous-dissolution device of monomer p-phenylene diamine in resin continuous polymerization process.
Background technology
Para-aramid fiber is a kind of high-performance fiber, has many superiority such as high intensity, high-modulus, high temperature resistant and solvent resistant
And can there is important application in national defence and civil area.Wherein continuous and stable production para-aramid fiber with poly-paraphenylene terephthalamide to benzene
Diamidogen (PPTA) resin is one of key therein.Industrial conventional PPTA polymerization is low-temperature solution polycondensation.I.e.
Monomer paraphthaloyl chloride (TPC) and p-phenylenediamine (PPD) are carried out low temperature polymerization reaction in suitable dicyandiamide solution.
Up to the present the existing substantial amounts of report about PPTA low temperature solution polymerization.But, how to realize extensive stable batch poly-
The report that symphysis is produced is the most few.
Wherein, the dissolving of monomer p-phenylene diamine and the mode of addition reaction are extremely important to realizing the polymerization of PPTA continuous-stable.Cause
Easily aoxidizing for PPD activity height, oxidation product the most all has stronger dyeability, so PPD dissolution mechanism is unreasonable, no
Only can affect the molecular weight of polymer P PTA, and the color and luster of polymerizate can be affected, and then para-aramid fiber can be affected
Quality.The most conventional PPD dissolves and processing mode has two kinds: one to be in solvent N-first by high-purity PPD elder generation stirring and dissolving
In base ketopyrrolidine (NMP), then cooling continues polyreaction with another monomer paraphthaloyl chloride；Two is to be added by PPD
Heat fusing, then with injection or other mode dispersing and dissolvings in NMP.Both approaches is problem for small lot batch manufacture
Not quite, but will be problematic for high-volume polymerization.Because both approaches is all batch dissolution PPD, PPD
After dissolving through long storage time can gradually variable color, even if having high pure nitrogen protection variable color also can occur.So batch (-type) dissolves PPD
Stability for keeping the PPTA resin of high-volume continuous and stable production is unfavorable.
Summary of the invention
To this end, the utility model proposes a kind of new p-phenylenediamine continuous-dissolution device, i.e. replace often with PPD continuous-dissolution
Batch (-type) dissolve so that all processes of PPTA polymerization are all continuous operations, and by by PPD continuous-dissolution,
Eliminate the PPD oxidation stain impact on PPTA quality stability, and then ensure that the stability of PPTA mass.
The continuous-dissolution device of a kind of p-phenylenediamine described in the utility model, including Weighing system, dissolution system, cooling system
And stocking system；
Described Weighing system includes feed bin；The all feed bins of Weighing system and pipeline high-purity nitrogen gas shielded；Weighing system can
Continuous-stable accurately measures PPD weight, preferred high accuracy Weightlessness balance.
Described dissolution system includes that continuous-dissolution still, continuous-dissolution still are provided with charging aperture, gas feed, discharging opening and gas
Body exports；Agitating device and grid it is provided with in continuous-dissolution still；Described agitating device includes motor, shaft and stirrer paddle；
Described grid is porous disc, is fixed on still wall；Shaft passes grid center, keeps 1-10mm gap with grid；
Described feed bin is connected with charging aperture by pipeline；
Described discharging opening is connected with cooling system and stocking system successively by pipeline.
Continuous-dissolution still can be vertical, it is also possible to is horizontal, the most horizontal.Blade is maintained at continuous-dissolution still wall gap
1-10mm, can stir solid PPD and don't can occur to be advisable with wall-friction.In order to control solution temperature, continuously
Dissolution kettle can the cooling of outer jacketed, it is also possible to need not, need not be preferred.Logical high pure nitrogen protection in continuous-dissolution still.Enter
Material mouth is located close to the continuous-dissolution still top of motor side, and discharging opening is positioned at bottom or the sidewall of the continuous-dissolution still other end,
Preferably sidewall discharging is to reduce the risk that solid PPD is carried over.If vertical dissolution kettle, agent set is still by agitating device
Forming with grid, simply charging aperture and High Purity Nitrogen blow vent change to top.
In order to ensure being completely dissolved of PPD, described continuous-dissolution still draw ratio is 5:1-10:1.
Cooling system described in the utility model uses industrial conventional vertical or horizontal heat exchanger.Control refrigerating capacity by molten
Material continuous coo1ing after solution is to the temperature of regulation.
Using device described in the utility model can realize the continuous-dissolution of p-phenylenediamine, it concretely comprises the following steps:
Nitrogen is passed through in whole device by air inlet, p-phenylenediamine powder is joined in the feed bin of weighing system, open and claim
Weight system continuous-stable adds p-phenylenediamine in continuous-dissolution still；Meanwhile, the N-that high-precision measuring pump will prepare is utilized
Methyl pyrrolidone/calcium chloride solution is transported in continuous-dissolution still by charging aperture continuous-stable；Open stirring of continuous-dissolution still
Mix, control rotating speed at 10-150rpm；Open out material conveying pump and the material dissolved be transported in cooling system be cooled to-5-5 DEG C,
Then the material storing cooled down will be dissolved to standby in stocking system.
In sum, in a kind of para-aramid fiber resin continuous polymerization process that the utility model proposes, monomer p-phenylene diamine is even
The continuous device dissolved, the auxiliary continuous-dissolution achieving PPD in corresponding manner.PPD eliminates PPD in the way of continuous-dissolution
The oxidation impact on PPTA resin quality, it is achieved that PPD dissolves the stability of quality, is possible not only to ensure PPTA molecular weight
Stablize, and can ensure that PPTA resin color consistency, thus lay solid base for follow-up aramid fiber quality stability
Plinth.
Accompanying drawing explanation
Fig. 1 is the continuous-dissolution apparatus structure schematic diagram of p-phenylenediamine described in the utility model；
In figure: 1, feed bin, 2, continuous-dissolution still, 3, charging aperture, 4, gas feed, 5, discharging opening, 6, gas outlet,
7, grid, 8, motor, 9, shaft, 10, stirrer paddle, 11, cooling system, 12, stocking system, 13, discharging defeated
Send pump.
Detailed description of the invention
Below by example, this utility model is further described, but content not thereby limiting the invention.
Embodiment 1
The continuous-dissolution device of a kind of p-phenylenediamine, this device includes Weighing system, dissolution system, cooling system and stocking system；
Described Weighing system includes feed bin 1；
Described dissolution system includes that continuous-dissolution still 2, continuous-dissolution still 2 are provided with charging aperture 3, gas feed 4, discharging opening
5 and gas outlet 6；Agitating device and grid 7 it is provided with in continuous-dissolution still 2；Described agitating device includes motor 8, stirs
Mix axle 9 and stirrer paddle 10；Described grid 7 is porous disc, is fixed on still wall；Shaft 9 passes grid 7 center,
1mm gap is kept with grid 7；
Described feed bin 1 is connected with charging aperture 3 by pipeline；
Described discharging opening 5 is connected with cooling system 11 and stocking system 12 successively by pipeline.
Described continuous-dissolution still 2 draw ratio is 5:1.
Described stirrer paddle 1 is maintained at 1mm with continuous-dissolution still wall gap.
The method utilizing the continuous-dissolution device continuous-dissolution p-phenylenediamine of above-mentioned p-phenylenediamine, it concretely comprises the following steps:
Nitrogen is passed through in whole device by air inlet 3, p-phenylenediamine powder is joined in the feed bin 1 of weighing system, open
Open weighing system continuous-stable in continuous-dissolution still 2, add p-phenylenediamine；Meanwhile, high-precision measuring pump is utilized to prepare
Good N-Methyl pyrrolidone/calcium chloride solution is transported in continuous-dissolution still 2 by charging aperture 3 continuous-stable；Open the most molten
Solve the stirring of still 2, control rotating speed at 10rpm；Open out material conveying pump 13 and the material dissolved is transported to cooling system 11
In be cooled to-5 DEG C, then will dissolve the material storing that cooled down to standby in stocking system 12.
PPD solution after dissolving and cooling down with reference to described in patent ZL201210485817.3 continuous polymerization method and another
Individual monomer TPC continuous polymerization, the PPTA powder determination of ubbelohde viscometer logarithmic specific concentration viscosity finally given is 6.20, accurate
Color difference meter continuous detecting PPTA toner, aberration is less than 0.02.
Embodiment 2
The continuous-dissolution device of a kind of p-phenylenediamine, this device includes Weighing system, dissolution system, cooling system and stocking system；
Described Weighing system includes feed bin 1；
Described dissolution system includes that continuous-dissolution still 2, continuous-dissolution still 2 are provided with charging aperture 3, gas feed 4, discharging opening
5 and gas outlet 6；Agitating device and grid 7 it is provided with in continuous-dissolution still 2；Described agitating device includes motor 8, stirs
Mix axle 9 and stirrer paddle 10；Described grid 7 is porous disc, is fixed on still wall；Shaft 9 passes grid 7 center,
10mm gap is kept with grid 7；
Described feed bin 1 is connected with charging aperture 3 by pipeline；
Described discharging opening 5 is connected with cooling system 11 and stocking system 12 successively by pipeline.
Described continuous-dissolution still 2 draw ratio is 10:1.
Described stirrer paddle 1 is maintained at 10mm with continuous-dissolution still wall gap.
The method utilizing the continuous-dissolution device continuous-dissolution p-phenylenediamine of above-mentioned p-phenylenediamine, it concretely comprises the following steps:
Nitrogen is passed through in whole device by air inlet 3, p-phenylenediamine powder is joined in the feed bin 1 of weighing system, open
Open weighing system continuous-stable in continuous-dissolution still 2, add p-phenylenediamine；Meanwhile, high-precision measuring pump is utilized to prepare
Good N-Methyl pyrrolidone/calcium chloride solution is transported in continuous-dissolution still 2 by charging aperture 3 continuous-stable；Open the most molten
Solve the stirring of still 2, control rotating speed at 150rpm；Open out material conveying pump 13 and the material dissolved is transported to cooling system 11
In be cooled to 5 DEG C, then will dissolve the material storing that cooled down to standby in stocking system 12.
PPD solution after dissolving and cooling down with reference to described in patent ZL201210485817.3 continuous polymerization method and another
Individual monomer TPC continuous polymerization, the PPTA powder determination of ubbelohde viscometer logarithmic specific concentration viscosity finally given is 5.5, accurate
Color difference meter continuous detecting PPTA toner, aberration is less than 0.02.
Embodiment 3
The continuous-dissolution device of a kind of p-phenylenediamine, this device includes Weighing system, dissolution system, cooling system and stocking system；
Described Weighing system includes feed bin 1；
Described dissolution system includes that continuous-dissolution still 2, continuous-dissolution still 2 are provided with charging aperture 3, gas feed 4, discharging opening
5 and gas outlet 6；Agitating device and grid 7 it is provided with in continuous-dissolution still 2；Described agitating device includes motor 8, stirs
Mix axle 9 and stirrer paddle 10；Described grid 7 is porous disc, is fixed on still wall；Shaft 9 passes grid 7 center,
5mm gap is kept with grid 7；
Described feed bin 1 is connected with charging aperture 3 by pipeline；
Described discharging opening 5 is connected with cooling system 11 and stocking system 12 successively by pipeline.
Described continuous-dissolution still 2 draw ratio is 8:1.
Described stirrer paddle 1 is maintained at 5mm with continuous-dissolution still wall gap.
The method utilizing the continuous-dissolution device continuous-dissolution p-phenylenediamine of above-mentioned p-phenylenediamine, it concretely comprises the following steps:
Nitrogen is passed through in whole device by air inlet 3, p-phenylenediamine powder is joined in the feed bin 1 of weighing system, open
Open weighing system continuous-stable in continuous-dissolution still 2, add p-phenylenediamine；Meanwhile, high-precision measuring pump is utilized to prepare
Good N-Methyl pyrrolidone/calcium chloride solution is transported in continuous-dissolution still 2 by charging aperture 3 continuous-stable；Open the most molten
Solve the stirring of still 2, control rotating speed at 100rpm；Open out material conveying pump 13 and the material dissolved is transported to cooling system 11
In be cooled to 0 DEG C, then will dissolve the material storing that cooled down to standby in stocking system 12.
PPD solution after dissolving and cooling down with reference to described in patent ZL201210485817.3 continuous polymerization method and another
Individual monomer TPC continuous polymerization, the PPTA powder determination of ubbelohde viscometer logarithmic specific concentration viscosity finally given is 7.07, accurate
Color difference meter continuous detecting PPTA toner, aberration is less than 0.02.
Claims (3)
1. the continuous-dissolution device of a p-phenylenediamine, it is characterised in that: this device includes Weighing system, dissolution system, cooling system and stocking system；
Described Weighing system includes feed bin (1)；
Described dissolution system includes that continuous-dissolution still (2), continuous-dissolution still (2) are provided with charging aperture (3), gas feed (4), discharging opening (5) and gas outlet (6)；Agitating device and grid (7) it is provided with in continuous-dissolution still (2)；Described agitating device includes motor (8), shaft (9) and stirrer paddle (10)；Described grid (7) is porous disc, is fixed on still wall；Shaft (9) passes grid (7) center, keeps 1-10mm gap with grid (7)；
Described feed bin (1) is connected with charging aperture (3) by pipeline；
Described discharging opening (5) is connected with cooling system (11) and stocking system (12) successively by pipeline.
The continuous-dissolution device of a kind of p-phenylenediamine the most according to claim 1, it is characterised in that: described continuous-dissolution still (2) draw ratio is 5:1-10:1.
The continuous-dissolution device of a kind of p-phenylenediamine the most according to claim 1 and 2, it is characterised in that: described stirrer paddle (10) and continuous-dissolution still wall gap are maintained at 1-10mm.
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| CN201620323856.7U CN205517338U (en) | 2016-04-18 | 2016-04-18 | P phenylenediamine's continuous dissolving device |
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| CN201620323856.7U CN205517338U (en) | 2016-04-18 | 2016-04-18 | P phenylenediamine's continuous dissolving device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688706A (en) * | 2016-04-18 | 2016-06-22 | 山东万圣博科技股份有限公司 | Continuous ursol dissolving device and method |
| CN109402744A (en) * | 2018-12-26 | 2019-03-01 | 蓝星（成都）新材料有限公司 | A kind of homogenization system and method for poly(p-phenylene terephthalamide) polymer |
| CN109912795A (en) * | 2019-01-16 | 2019-06-21 | 河南神马尼龙化工有限责任公司 | A kind of production method and PPD dissolution kettle of high-quality poly(p-phenylene terephthalamide) resin |
| CN110684192A (en) * | 2019-11-07 | 2020-01-14 | 蓝星（成都）新材料有限公司 | P-phenylenediamine dissolving system and method for continuous polymerization of aramid fibers 1414 |
-
2016
- 2016-04-18 CN CN201620323856.7U patent/CN205517338U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688706A (en) * | 2016-04-18 | 2016-06-22 | 山东万圣博科技股份有限公司 | Continuous ursol dissolving device and method |
| WO2017181761A1 (en) * | 2016-04-18 | 2017-10-26 | 山东万圣博科技股份有限公司 | Apparatus and method for continuous melting of phenylenediamine |
| CN109402744A (en) * | 2018-12-26 | 2019-03-01 | 蓝星（成都）新材料有限公司 | A kind of homogenization system and method for poly(p-phenylene terephthalamide) polymer |
| CN109912795A (en) * | 2019-01-16 | 2019-06-21 | 河南神马尼龙化工有限责任公司 | A kind of production method and PPD dissolution kettle of high-quality poly(p-phenylene terephthalamide) resin |
| CN109912795B (en) * | 2019-01-16 | 2021-07-02 | 河南神马尼龙化工有限责任公司 | Production method of high-quality poly (p-phenylene terephthalamide) resin and PPD dissolving kettle |
| CN110684192A (en) * | 2019-11-07 | 2020-01-14 | 蓝星（成都）新材料有限公司 | P-phenylenediamine dissolving system and method for continuous polymerization of aramid fibers 1414 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 257300 Guangrao Binhai New Area in Dongying, Shandong Co-patentee after: Tsinghua University Patentee after: Zhongfang Special Fiber Co., Ltd. Address before: 257300 Guangrao Binhai New Area in Dongying, Shandong Co-patentee before: Tsinghua University Patentee before: Shandong Wanshengbo Technology Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |