CN102775600B - Polymerization manufacturing technique and device for polyamide - Google Patents
Polymerization manufacturing technique and device for polyamide Download PDFInfo
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Abstract
The invention relates to a polymerization manufacturing technique and device for polyamide. The manufacturing technique comprises the steps of feeding molten caprolactam, titanium dioxide, benzoic acid and an additive, dynamically mixing at a high temperature for prepolymerization and postpolymerization, granulating, pre-extracting, extracting and drying to obtain the final product. The device comprises a melting system, a feed system, a high-temperature dynamic mixing system, prepolymerization and postpolymerization towers, a pre-extraction column, an extraction column, a recycling system and a drying tower. According to the invention, a high-temperature dynamic mixing tank is set additionally. The mixing of the raw materials and hydrolysis for ring opening and dehydration of polyamide are performed at a state of dynamically mixing to achieve a more sufficient and stable pre-addition polymerization and a more uniform and stable molecular distribution of post-polycondensation. A slice and a water separator of the extraction column are used for mainly extracting oligomers through the pre-extraction column and extracting a caprolactam monomer through the extraction column with a stable concentration. A slice cooler of the drying tower is used for cooling the slices rapidly. An extraction water recycling system is used for recycling the oligomers in the pre-extraction water and the caprolactam monomer in the extraction water.
Description
Technical field
The present invention relates to the Processes and apparatus that a kind of polymerizing polyamide is produced.
Background technology
China is mainly to quote import equipment and external advanced technologies for the continuous synthetic fibre 6 section polymerization techniques of polymeric amide at present, and it mainly contains Ji Ma, Yi Wenda-card Fischer, A Jiafei, noy etc.And the equipment and process of introducing is all had no idea for high-end civilian high-speed spinning section, will be more obvious in particular for high-end thin dawn spinning chips problem, the section of producing can only be cut into slices for the production of routine section and low side engineering plastics, thereby caused, domesticly for high-end civilian section, mainly still relies on import.Import equipment is partly comprised of caprolactam melting device, titanium dioxide dispenser, phenylformic acid dispenser, caprolactam charging stock tank, pre-polymerization tower, post polymerization tower, dicing machine, extraction tower, drying tower and conveying and packaging, and whole system adopts DCS automatization to control.Polymerizing polyamide production technique is hexanolactam charging together with titanium dioxide, phenylformic acid of melting, through pre-polymerization, post polymerization, pelletizing, extraction, the dry product that to obtain.
Following three subject matters that the polymerization technique of introducing at present and equipment exist:
1, polyreaction molecular weight distribution is out too wide, and the change of molecular weight is large;
2, there is the oxidized phenomenon of section and the extraction of oligomers problem of having no idea in extracting system;
3, drying temperature is too high, and chip drying adopts high temperature drying greatly to increase the solid-phase tack producing of section
Spinning property and the spinning intensity of the 1st problem major effect section, easily cause the unstable of filament spinning component; There is a large amount of dead angles mainly due to extracting system in the 2nd problem, section motion is inhomogeneous causes a large amount of Huangs to cut into slices; The 3rd problem drying temperature height easily causes section oxidation viscose glue, will produce so a large amount of viscose glue particles, makes spinning produce a large amount of waft silk and broken end, the directly spinning property of impact section.
For addressing the above problem, the applicant has < < polymerizing polyamide production technology and equipments > > (China Patent No. 200710052102.8) patent, by caprolactam melting, the hexanolactam of melting and titanium dioxide, phenylformic acid is charging together, through pre-polymerization, post polymerization, pelletizing, extraction, be dried to obtain product, caprolactam melting adopts nitrogen-sealed, the preparation of employing de-salted water, the hexanolactam of melting and titanium dioxide, phenylformic acid filters with standard fine filter, enter caprolactam feed system, through pre-polymerization, post polymerization, pelletizing, extraction, be dried under Full-closed system and nitrogen protection and carry out.
Polymerizing polyamide production unit, the heating tubulation of the polymerizing pipe epimere of post polymerization tower is caught up with face honeybee shape dividing plate johning knot and is combined, and hypomere has heating coil subassembly;
Extraction tower has steam companions, section extraction sparger outward, tower top has header tank, under have annulus inlet distribution device, annulus inlet distribution device bottom is taper, the cone bucket that section extraction sparger is a plurality of stacks, cone bucket consists of inverted trapezoidal cone and right circular cone, and space is left in centre, and it is 8-20mm macropore that inverted trapezoidal cone top is uniformly distributed aperture.
Drying tower has cone bucket up and down, cone bucket consists of inverted trapezoidal cone and right circular cone, in the middle of inverted trapezoidal cone and right circular cone, leave space, water conservancy diversion venting hole is arranged at right circular cone top, water conservancy diversion venting hole aperture 40-80mm, between inverted trapezoidal cone and top cylindrical shell, bottom cylindrical shell, have the nitrogen air supplying ring being communicated with nitrogen blast inlet, the diameter of drying tower top cylindrical shell is greater than the diameter of bottom cylindrical shell.
Though this patent has solved the problem of solid-phase tack producing, also improved interior quality and the quality of section simultaneously, also do not have oligomer extraction problem and the caprolactam monomer in extraction water in fine solution section to reclaim problem.
Summary of the invention
The object of the invention is for above-mentioned present situation, aim to provide a kind of solid-phase tack producing and the oligomer that can effectively control in dry sliced, effectively promote slicing product quality, the polymerizing polyamide production technology and equipments of the caprolactam monomer in efficient recovery extraction water.
The implementation of the object of the invention is; polymerizing polyamide production technique; caprolactam melting; the charging together with titanium dioxide, phenylformic acid, additive of the hexanolactam of melting; after high temperature dynamically mixes, carry out pre-polymerization, post polymerization, pre-extraction, extraction, pelletizing, be dried to obtain product; pelletizing, pre-extraction, extraction, drying process are carried out under Full-closed system and nitrogen protection
Caprolactam melting adopts de-salted water preparation, is formulated under nitrogen-sealed protection and carries out, and the hexanolactam of melting and titanium dioxide, phenylformic acid, additive filter with standard fine filter, enter caprolactam feed system,
The dosage of titanium dioxide, phenylformic acid, additive is respectively 2.0-2.5 ‰, 1.2-1.5 ‰, the 1.2-1.5 ‰ of hexanolactam weight,
Described additive is 2,2,6,6-tetramethyl--4-amino piperidine, 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid, one or more in 3-diethyl propylamine and two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
Polymerizing polyamide production unit, have caprolactam fusing system, titanium dioxide compounding system, phenylformic acid compounding system, caprolactam feed system, pre-polymerization tower, post polymerization tower, pelletizing system, extraction tower, drying tower, extraction water recovery system and conveying and packaging system, whole system adopts DCS automatization to control;
The heating tubulation of the polymerizing pipe epimere of post polymerization tower is caught up with face honeybee shape dividing plate johning knot and is combined, and hypomere has heating coil subassembly;
Extraction tower has steam companions outward, inside there is section extraction sparger, tower top has header tank, under have annulus inlet distribution device, annulus inlet distribution device bottom is taper, the cone bucket that section extraction sparger is a plurality of stacks, and cone bucket consists of inverted trapezoidal cone and right circular cone, space is left in centre, and it is 8-20mm macropore that inverted trapezoidal cone top is uniformly distributed aperture;
Drying tower has cone bucket up and down, cone bucket consists of inverted trapezoidal cone and right circular cone, in the middle of inverted trapezoidal cone and right circular cone, leave space, water conservancy diversion venting hole is arranged at right circular cone top, water conservancy diversion venting hole aperture 40-80mm, between inverted trapezoidal cone and top cylindrical shell, bottom cylindrical shell, have the nitrogen air supplying ring being communicated with nitrogen blast inlet, the diameter of drying tower top cylindrical shell is greater than the diameter of bottom cylindrical shell;
There are the dynamic mixing tank of high temperature, the dynamic mixing tank of high temperature to have agitator, top to be provided with bubble-cap, have heating semicanal outward, inside have spiral heater;
Pre-extraction tower top is provided with blanking conduit, and bottom is provided with pre-extraction dope charging distributing slot; The overflow port of pre-extraction tower connects extraction water recovery system;
On the header tank top of extraction tower tower top, have section, water separator, in section, water separator, have section water separate mesh, section, water separator are communicated with header tank; The overflow port of extraction tower connects extraction water recovery system;
Drying tower bottom cylindrical shell is provided with section water cooler, and section condenser connects conveying and packaging system.
The present invention increases the dynamic hybrid technique of high temperature and the dynamic mixing tank of high temperature on former patent basis, raw material mixes and polymeric amide hydrolysis, dehydration, under the dynamic admixture of high temperature, carry out, make its reaction more evenly, more fully, dewater faster, make pre-polymerization polyaddition reaction more fully, more stable; Post polymerization polycondensation phase molecular distribution more evenly, more stable.Upper section, the water separator of increasing in extraction tower tower top header tank top, make the pre-extraction tower and the extraction tower definite functions that newly increase, pre-extraction water and extraction water are independent of each other, effectively control and regulate in pre-extraction water and extraction water the stable of concentration separately, reach pre-extraction tower emphasis extraction of oligomers, the object of extraction tower emphasis extraction caprolactam monomer.Drying tower bottom cylindrical shell is provided with section water cooler, and the dry sliced temperature of leaving after drying tower of fast reducing prevents that section is oxidized in discharge and wrapping process; Pre-extraction tower and extraction tower connect pre-extraction water and extraction water recovery system, process the oligopolymer reclaiming in pre-extraction water, after the caprolactam monomer in extraction water, then iterative cycles use, reach zero release.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention,
Fig. 2 is the dynamic mixing tank structural representation of high temperature,
Fig. 3 is post polymerization tower structure schematic diagram,
Fig. 4 is pre-extraction tower structural representation,
Fig. 5 is extraction tower structural representation,
Fig. 6 is drying tower structural representation.
Embodiment
With reference to Fig. 1, polymerization process flow process of the present invention is: caprolactam melting, pre-polymerization, post polymerization, pelletizing, pre-extraction, extraction, extraction water recovery, the dry product that to obtain are carried out in the charging together with titanium dioxide, phenylformic acid, additive of the hexanolactam of melting after high temperature dynamically mixes.Pre-extraction water, extraction water after pre-extraction, extraction process through extraction water recovery system the oligopolymer reclaiming in pre-extraction water, after the caprolactam monomer in extraction water, recycle.
Polymerization production unit of the present invention is partly comprised of hexanolactam fusing system, titanium dioxide compounding system, phenylformic acid compounding system, additive compounding system, hexanolactam feed system, the dynamic mixing system of high temperature, pre-polymerization tower, post polymerization tower, pelletizing system, pre-extracting system, extraction tower, extraction water recovery system, drying tower and conveying and packaging.Production unit of the present invention is described in detail in detail with reference to the accompanying drawings.
With reference to Fig. 2, carrying out the dynamic dynamic mixing tank 1 of high temperature mixing of high temperature of the present invention has agitator 2, top to be provided with bubble-cap 3, has heating semicanal 5 outward, inside has spiral heater 4.The present invention mixes and polymeric amide hydrolysis, dehydration the hexanolactam of melting and titanium dioxide, phenylformic acid, additive, under the dynamic admixture of high temperature, carries out, make its reaction more evenly, more fully, dewater faster.Make pre-polymerization polyaddition reaction more fully, more stable, be also conducive to simultaneously post polymerization polycondensation phase molecule branch more evenly, more stable.
With reference to Fig. 3, the heating tubulation 8 of polymerizing pipe 6 epimeres of post polymerization tower is caught up with face honeybee shape dividing plate 9 johning knots and is combined, hypomere has heating coil subassembly 7, increase post polymerization midsection heat interchanging area, energy quick adjustment polymerization tower stage casing temperature, increase the hypomere polycondensation equilibrium time, extend the starting time of polymer molecule, increase the homogeneity of molecular weight, make polyreaction more even, more stable, to reach the technical requirements of high-speed spinning section.
With reference to Fig. 4, pre-extraction tower 10 tops are provided with blanking conduit 11, and bottom is provided with pre-extraction dope charging distributing slot 12, and the overflow port 28 of pre-extraction tower connects extraction water recovery system.The present invention increases pre-extraction tower newly, pre-extraction tower is completely different from the extraction tower function shown in Fig. 5, extraction tower can only extract the caprolactam monomer in section, and section in oligopolymer cannot extract, oligopolymer only has by pre-extraction tower, and certain density caprolactam water solution is extracted.Oligopolymer in pre-extraction tower extraction section, thus oligopolymer, viscose glue particle and the monomer content in section effectively controlled, guarantee chipping qualities.
With reference to Fig. 5, extraction tower 14 is outer have steam companions 18, in have section extraction sparger 16, tower top has header tank 13, under have annulus inlet distribution device 17, annulus inlet distribution device bottom is taper.The cone bucket that section extraction sparger is a plurality of stacks, cone bucket consists of inverted trapezoidal cone and right circular cone, and space is left in centre.It is 8-20mm macropore that inverted trapezoidal cone top is uniformly distributed aperture.Header tank has section, water separator 19 on 13 tops, in section, water separator, has section water separate mesh 20.Section, water separator are communicated with header tank 13, and the overflow port 29 of extraction tower connects extraction water recovery system.
The present invention sets up section, water separator 19 on header tank 13 tops, in section, water separator, has section water separate mesh 20.Section, water separator are connected with header tank 13.Can make so pre-extraction tower and extraction tower definite functions, pre-extraction water and extraction water are independent of each other, effectively control and regulate in pre-extraction water and extraction water the stable of concentration separately.
With reference to Fig. 6, drying tower 21 has cone bucket up and down, and cone bucket consists of inverted trapezoidal cone 26 and right circular cone 22, in the middle of inverted trapezoidal cone 26 and right circular cone 22, leaves space.Water conservancy diversion venting hole is arranged at right circular cone top, water conservancy diversion venting hole aperture 40-80mm, and inverted trapezoidal cone 26 has with top cylindrical shell 21,24 of bottom cylindrical shells the nitrogen air supplying ring being communicated with nitrogen blast inlet 23.The diameter of drying tower top cylindrical shell 21 is greater than the diameter of bottom cylindrical shell 24.Bottom cylindrical shell 24 is provided with section water cooler 27.
The present invention sets up section water cooler 27 for 24 times at bottom cylindrical shell, and the dry sliced temperature of leaving after drying tower of energy fast reducing prevents that section is oxidized in discharge and wrapping process.Pre-extraction tower and extraction tower connect extraction water recovery system, process the oligopolymer reclaiming in pre-extraction water, and after the caprolactam monomer in extraction water, recirculation is used, and reaches zero release.
With specific embodiment in detail the present invention is described in detail below.
Example 1, caprolactam adopts de-salted water preparation in caprolactam fusing system, be formulated in melting under nitrogen-sealed, the hexanolactam of melting enters caprolactam feed system, by titanium dioxide compounding system, prepared, its weight is the titanium dioxide of caprolactam 2.0 ‰, by phenylformic acid configurator, prepared, weight is caprolactam 1.2 ‰ phenylformic acid and 1.2 ‰ pairs (2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphites filters with standard fine filter, enter together caprolactam feed system, send into the dynamic mixing tank of high temperature, after dynamically mixing, high temperature carries out pre-polymerization tower, after the polymerization of post polymerization tower, Qie La, by blanking conduit 11, enter pre-extraction tower, oligopolymer in extraction section, then by section, section water separate mesh 20 in water separator 19 enters extraction tower, caprolactam monomer in extraction section, dehydration, drying tower is dry, again through the cooling product that obtains of section water cooler 27.Pelletizing, pre-extraction, extraction, drying process are carried out under Full-closed system and nitrogen protection.
Example 2, with example 1, different is, by titanium dioxide compounding system, prepared, the titanium dioxide of its weight 2.5 ‰, 1.5 ‰ phenylformic acid and 0.5 ‰ 2 of being prepared by phenylformic acid configurator, 2,6,6-tetramethyl--4-amino piperidine, 0.3 ‰ 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid and standard fine filter filtration for 0.5 ‰ 3-diethyl propylamine.
Example 3, with example 1, different is, by titanium dioxide compounding system, prepared, the titanium dioxide of its weight 2.5 ‰, 1.5 ‰ phenylformic acid and 0.3 ‰ 2 of being prepared by phenylformic acid dispenser, 2,6,6-tetramethyl--4-amino piperidine, 0.3 ‰ 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid and standard fine filter filtration for 0.6 ‰ 3-diethyl propylamine.
Example 3, with example 1, different is, by titanium dioxide compounding system, prepared, the titanium dioxide of its weight 2.5 ‰, 1.5 ‰ phenylformic acid and 0.3 ‰ 2 of being prepared by phenylformic acid dispenser, 2,6,6-tetramethyl--4-amino piperidine, 0.4 ‰ 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid, 0.4 ‰ 3-diethyl propylamine and 0.4 ‰ pairs of (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites filter with standard fine filter.
Claims (2)
1. polymerizing polyamide production technique; caprolactam melting; it is characterized in that hexanolactam charging together with titanium dioxide, phenylformic acid, additive of melting; after high temperature dynamically mixes, carry out pre-polymerization, post polymerization, pre-extraction, extraction, pelletizing, be dried to obtain product; pelletizing, pre-extraction, extraction, drying process are carried out under Full-closed system and nitrogen protection
Caprolactam melting adopts de-salted water preparation, is formulated under nitrogen-sealed and carries out, and the hexanolactam of melting and titanium dioxide, phenylformic acid, additive filter with standard fine filter, enter caprolactam feed system,
The dosage of titanium dioxide, phenylformic acid, additive is respectively 2.0-2.5 ‰, 1.2-1.5 ‰, the 1.2-1.5 ‰ of hexanolactam weight,
Described additive is 2,2,6,6-tetramethyl--4-amino piperidine, 3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid, one or more in 3-diethyl propylamine and two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
2. adopt the equipment of the polymerization process production polymeric amide of claim 1, have caprolactam fusing system, titanium dioxide compounding system, phenylformic acid compounding system, caprolactam feed system, pre-polymerization tower, post polymerization tower, pelletizing system, extraction tower, drying tower, extraction water recovery system and conveying and packaging system, whole system adopts DCS automatization to control;
The heating tubulation of the polymerizing pipe epimere of post polymerization tower is caught up with face honeybee shape dividing plate johning knot and is combined, and hypomere has heating coil subassembly;
Extraction tower has steam companions outward, inside there is section extraction sparger, tower top has header tank, under have annulus inlet distribution device, annulus inlet distribution device bottom is taper, the cone bucket that section extraction sparger is a plurality of stacks, and cone bucket consists of inverted trapezoidal cone and right circular cone, space is left in centre, and it is 8-20mm macropore that inverted trapezoidal cone top is uniformly distributed aperture;
Drying tower has cone bucket up and down, cone bucket consists of inverted trapezoidal cone and right circular cone, in the middle of inverted trapezoidal cone and right circular cone, leave space, water conservancy diversion venting hole is arranged at right circular cone top, water conservancy diversion venting hole aperture 40-80mm, between inverted trapezoidal cone and top cylindrical shell, bottom cylindrical shell, have the nitrogen air supplying ring being communicated with nitrogen blast inlet, the diameter of drying tower top cylindrical shell is greater than the diameter of bottom cylindrical shell;
It is characterized in that having the dynamic mixing tank of high temperature, the dynamic mixing tank of high temperature to have agitator, top to be provided with bubble-cap, have heating semicanal outward, inside have spiral heater;
Pre-extraction tower top is provided with blanking conduit, and bottom is provided with pre-extraction dope charging distributing slot; The overflow port of pre-extraction tower connects extraction water recovery system;
On the header tank top of extraction tower tower top, have section, water separator, in section, water separator, have section water separate mesh, section, water separator are communicated with header tank; The overflow port of extraction tower connects extraction water recovery system;
Drying tower bottom cylindrical shell is provided with section water cooler, and section water cooler connects conveying and packaging system.
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| CN105801842A (en) * | 2016-04-20 | 2016-07-27 | 温州邦鹿化工有限公司 | Polyamide polymerization production technology |
| CN105820331A (en) * | 2016-04-20 | 2016-08-03 | 温州邦鹿化工有限公司 | Polyamide polymerization production process |
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