CN102775600A - Polymerization manufacturing technique and device for polyamide - Google Patents
Polymerization manufacturing technique and device for polyamide Download PDFInfo
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- CN102775600A CN102775600A CN2012102718169A CN201210271816A CN102775600A CN 102775600 A CN102775600 A CN 102775600A CN 2012102718169 A CN2012102718169 A CN 2012102718169A CN 201210271816 A CN201210271816 A CN 201210271816A CN 102775600 A CN102775600 A CN 102775600A
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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
It mainly is to quote import equipment and external advanced technologies that present China is used for the continuous synthetic fibre 6 section polymerization techniques of polymeric amide, and it mainly contains Ji Ma, Yi Wenda-card Fischer, A Jiafei, noy etc.And equipment of introducing and technology all have no idea to be used 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 used to produce conventional section cuts into slices with the low side engineering plastics, domesticly is used for high-end civilian section and mainly still relies on import thereby caused.Import equipment partly is made up of caprolactam melting device, titanium oxide 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 total system adopts DCS robotization control.The polymerizing polyamide production technique is that the fused hexanolactam is with titanium oxide, phenylformic acid charging, through pre-polymerization, post polymerization, pelletizing, extraction, the dry product that gets.
Following three subject matters that polymerization technique of introducing at present and equipment exist:
1, the polyreaction MWD of coming out is too wide, and molecular weight changes greatly;
2, extracting system exists the oxidized phenomenon of section and the extraction of oligomers problem of having no idea;
3, drying temperature is too high, and chip drying adopts high temperature drying to increase the solid-phase tack producing of section greatly
The 1st problem mainly influences the spinning property and the spinning intensity of section, causes the instability of filament spinning component easily; There is a large amount of dead angles in the 2nd problem mainly due to extracting system, and the section motion is inhomogeneous to cause a large amount of Huangs to cut into slices; The 3rd problem drying temperature height causes section oxidation viscose glue easily, will produce a large amount of viscose glue particles like this, makes spinning produce a large amount of waft silk and broken end, the directly spinning property of influence section.
For addressing the above problem, the applicant has " polymerizing polyamide production technique and equipment " (Chinese patent number 200710052102.8) patent, is with the caprolactam fusion; The fused hexanolactam is with titanium oxide, phenylformic acid charging; Through pre-polymerization, post polymerization, pelletizing, extraction, the dry product that gets, nitrogen-sealed is adopted in the caprolactam fusion, adopts the de-salted water preparation; Fused hexanolactam and titanium oxide, phenylformic acid filter with the standard fine filter; Enter the caprolactam feed system, through pre-polymerization, post polymerization, pelletizing, extraction, drying are carried out under hermetically sealed system and nitrogen protection.
Polymerizing polyamide production unit, the heating tubulation of the polymerizing pipe epimere of post polymerization tower are caught up with face honeybee shape dividing plate johning knot and are lumped together, and hypomere has the heating coil subassembly;
Extraction tower has steam companions, section extraction sparger outward; Cat head has header tank, down annulus inlet distribution device is arranged, and annulus inlet distribution device bottom is taper; Section extraction sparger is a plurality of synergetic awl buckets; Awl bucket constitutes by falling trapezoidal cone and right circular cone, and the space is left in the centre, and falling uniform distribution aperture, trapezoidal cone top is the 8-20mm macropore.
Drying tower has the awl bucket up and down; Awl bucket constitutes by falling trapezoidal cone and right circular cone; Fall and leave the space in the middle of trapezoidal cone and the right circular cone, the water conservancy diversion venting hole is arranged at the right circular cone top, water conservancy diversion venting hole aperture 40-80mm; Falling has the nitrogen air supplying ring that is communicated with the nitrogen blast inlet between trapezoidal cone and top cylindrical shell, bottom cylindrical shell, and 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 the interior quality and the quality of section simultaneously, also there are not oligomer extraction problem and the caprolactam monomer in the extraction water in the fine solution section to reclaim problem.
Summary of the invention
The objective of the invention is to above-mentioned present situation; Aim to provide a kind of solid-phase tack producing and the oligomer that can control effectively in dry sliced; Effectively promote slicing product quality, the polymerizing polyamide production technique and the equipment of the caprolactam monomer in the efficient recovery extraction water.
The implementation of the object of the invention does; The polymerizing polyamide production technique; Caprolactam fusion, fused hexanolactam are carried out pre-polymerization, post polymerization, extraction in advance, extraction, pelletizing, the dry product that gets with titanium oxide, phenylformic acid, additive charging after high temperature dynamically mixes; Pelletizing, extraction in advance, extraction, drying process are carried out under hermetically sealed system and nitrogen protection
The de-salted water preparation is adopted in the caprolactam fusion, is formulated under the nitrogen-sealed protection to carry out, and fused hexanolactam and titanium oxide, phenylformic acid, additive filter with the standard fine filter, enter the caprolactam feed system,
The dosage of titanium oxide, phenylformic acid, additive is respectively 2.0-2.5 ‰, 1.2-1.5 ‰, the 1.2-1.5 ‰ of hexanolactam weight,
Said additive is 2,2,6,6-tetramethyl--4-amino piperidine, 3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid, one or more in 3-diethylammonium propylamine and two (2, the 4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
The polymerizing polyamide production unit; Caprolactam fusing system, titanium oxide 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 are arranged, and total system adopts DCS robotization 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 lumped together, and hypomere has the heating coil subassembly;
Extraction tower has steam companions outward, in section extraction sparger is arranged, cat head has header tank; Under annulus inlet distribution device is arranged; Annulus inlet distribution device bottom is taper, and section extraction sparger is a plurality of synergetic awl buckets, and the awl bucket constitutes by falling trapezoidal cone and right circular cone; The space is left in the centre, and falling uniform distribution aperture, trapezoidal cone top is the 8-20mm macropore;
Drying tower has the awl bucket up and down; Awl bucket constitutes by falling trapezoidal cone and right circular cone; Fall and leave the space in the middle of trapezoidal cone and the right circular cone, the water conservancy diversion venting hole is arranged at the right circular cone top, water conservancy diversion venting hole aperture 40-80mm; Falling has the nitrogen air supplying ring that is communicated with the nitrogen blast inlet between trapezoidal cone and top cylindrical shell, bottom cylindrical shell, and the diameter of drying tower top cylindrical shell is greater than the diameter of bottom cylindrical shell;
Have the dynamic mixing tank of high temperature, the dynamic mixing tank of high temperature to have whisking appliance, top to be provided with bubble-cap, the heating semicanal arranged outward, in spiral heater is arranged;
Extraction tower top is provided with the blanking conduit in advance, and the bottom is provided with preparatory collection dope charging distributing slot; The riser of extraction tower connects the extraction water recovery system in advance;
On the header tank top of extraction tower cat head section, water separator are arranged, section water sepn net is arranged in section, the water separator, section, water separator are communicated with header tank; The riser of extraction tower connects the extraction water recovery system;
Drying tower bottom cylindrical shell is provided with the section water cooler, and the section condensing surface meets the conveying and packaging system.
The present invention increases dynamic hybrid technique of high temperature and the dynamic mixing tank of high temperature on former patent basis; Raw materials mix and polymeric amide hydrolysis, dehydration; Under the dynamic admixture of high temperature, carry out; Make its reaction more evenly, more fully, dehydration is faster, make the pre-polymerization polyaddition reaction more fully, more stable; Post polymerization polycondensation phase molecular distribution more evenly, more stable.Go up on extraction tower cat head header tank top increases section, water separator; Make the preparatory extraction tower and the extraction tower definite functions that increase newly; Preparatory extraction water and extraction water are independent of each other; Effectively control and regulate in preparatory extraction water and the extraction water steady concentration separately, reach preparatory extraction tower emphasis extraction of oligomers, the purpose of extraction tower emphasis extraction caprolactam monomer.Drying tower bottom cylindrical shell is provided with the section water cooler, reduces the dry sliced temperature of leaving behind the drying tower fast, prevents section oxidation in discharging and wrapping process; Extraction tower and extraction tower connect preparatory extraction water and extraction water recovery system in advance, handle the oligopolymer that reclaims in the preparatory extraction water, behind the caprolactam monomer in the extraction water, recycle repeatedly again, reach zero release.
Description of drawings
Fig. 1 is a process flow sheet of the present invention,
Fig. 2 is the dynamic mixing tank structural representation of high temperature,
Fig. 3 is a post polymerization tower structure synoptic diagram,
Fig. 4 is preparatory extraction tower structural representation,
Fig. 5 is the extraction tower structural representation,
Fig. 6 is the drying tower structural representation.
Embodiment
With reference to Fig. 1; Polymerization process flow process of the present invention is: the caprolactam fusion; The fused hexanolactam carries out pre-polymerization, post polymerization, pelletizing, extraction in advance, extraction, extraction water recovery, the dry product that gets with titanium oxide, phenylformic acid, additive charging after high temperature dynamically mixes.Preparatory extraction water, extraction water after extraction in advance, the extraction are handled the oligopolymer that reclaims in the preparatory extraction water through the extraction water recovery system, recycle behind the caprolactam monomer in the extraction water.
Polymerization production unit of the present invention partly is made up of hexanolactam fusing system, titanium oxide 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, preparatory extracting system, extraction tower, extraction water recovery system, drying tower and conveying and packaging.Production unit of the present invention is detailed with reference to the accompanying drawings.
With reference to Fig. 2, carrying out the dynamic mixing tank 1 of the dynamic blended high temperature of high temperature of the present invention has whisking appliance 2, top to be provided with bubble-cap 3, have outward the heating semicanal 5, in spiral heater 4 is arranged.The present invention mixes and polymeric amide hydrolysis, dehydration fused hexanolactam and titanium oxide, phenylformic acid, additive, under the dynamic admixture of high temperature, carries out, make its reaction more evenly, more fully, dehydration is faster.Make the pre-polymerization polyaddition reaction more fully, more stable, also help 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 lumped together, and hypomere has heating coil subassembly 7; Increase post polymerization midsection heat interchanging area, ability quick adjustment polymerization tower stage casing temperature, increase the hypomere polycondensation equilibrium time, prolong 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, extraction tower 10 tops are provided with blanking conduit 11 in advance, and the bottom is provided with preparatory collection dope charging distributing slot 12, and the riser 28 of extraction tower connects the extraction water recovery system in advance.The present invention increases preparatory extraction tower newly; Extraction tower is different fully with extraction tower function shown in Figure 5 in advance; Extraction tower can only extract the caprolactam monomer in the section; And the oligopolymer in the section can't extract, and oligopolymer has only through in the preparatory extraction tower, and certain density caprolactam water solution extracts it.Oligopolymer during the extraction tower extraction is cut into slices in advance, thus oligopolymer, viscose glue particle and the monomer content in the section effectively controlled, guarantee chipping qualities.
With reference to Fig. 5, extraction tower 14 is outer have steam companions 18, in section extraction sparger 16 is arranged, cat head has header tank 13, down annulus inlet distribution device 17 is arranged, annulus inlet distribution device bottom is taper.Section extraction sparger is a plurality of synergetic awl buckets, and the awl bucket constitutes by falling trapezoidal cone and right circular cone, and the space is left in the centre.Falling uniform distribution aperture, trapezoidal cone top is the 8-20mm macropore.Header tank has section, water separator 19 on 13 tops, and section water sepn net 20 is arranged in section, the water separator.Section, water separator are communicated with header tank 13, and the riser 29 of extraction tower connects the extraction water recovery system.
The present invention sets up section, water separator 19 on header tank 13 tops, section water sepn net 20 is arranged in section, the water separator.Section, water separator are connected with header tank 13.Can make preparatory extraction tower and extraction tower definite functions like this, preparatory extraction water and extraction water are independent of each other, effectively control and regulate in preparatory extraction water and the extraction water steady concentration separately.
With reference to Fig. 6, drying tower 21 has awl bucket up and down, and the awl bucket constitutes with right circular cone 22 by falling trapezoidal cone 26, falls and leaves spaces in the middle of trapezoidal cone 26 and the right circular cone 22.The water conservancy diversion venting hole is arranged at the right circular cone top, water conservancy diversion venting hole aperture 40-80mm, and the trapezoidal cone 26 of falling has the nitrogen air supplying ring that is communicated with nitrogen blast inlet 23 with top cylindrical shell 21,24 of bottom cylindrical shells.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 in the bottom cylindrical shell set up section water cooler 27 for 24 times, can reduce the dry sliced temperature of leaving behind the drying tower fast, prevent section oxidation in discharging and wrapping process.Extraction tower and extraction tower connect the extraction water recovery system in advance, handle the oligopolymer that reclaims in the preparatory extraction water, and behind the caprolactam monomer in the extraction water, recycling is used, and reaches zero release.
With specific embodiment the present invention is detailed below.
Example 1, caprolactam adopt the de-salted water preparation in the caprolactam fusing system, be formulated in fusion under the nitrogen-sealed, and the fused hexanolactam gets into the caprolactam feed system; By titanium oxide compounding system preparation, its weight is the titanium oxide of caprolactam 2.0 ‰, by the preparation of phenylformic acid configurator, and weight is caprolactam 1.2 ‰ phenylformic acid and 1.2 ‰ pairs (2; The 4-di-tert-butyl-phenyl) pentaerythritol diphosphites filters with the standard fine filter, enters the caprolactam feed system together, sends into the dynamic mixing tank of high temperature; After after high temperature dynamically mixes, carrying out pre-polymerization tower, the polymerization of post polymerization tower, Qie La gets into preparatory extraction tower by blanking conduit 11; Oligopolymer in the extraction section; Then get into extraction tower, the caprolactam monomer in the extraction section, dehydration through the section water sepn net in section, the water separator 19 20; Dry through drying tower, again through section water cooler 27 cool off product.Pelletizing, extraction in advance, extraction, drying process are carried out under hermetically sealed system and nitrogen protection.
Routine 2, together routine 1; Different is, by the preparation of titanium oxide compounding system, and the titanium oxide of its weight 2.5 ‰, by 1.5 ‰ phenylformic acid and 0.5 ‰ 2 of phenylformic acid configurator preparation; 2; 6,6-tetramethyl--4-amino piperidine, 0.3 ‰ 3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid and 0.5 ‰ 3-diethylammonium propylamine filter with the standard fine filter.
Example 3, same example 1, different is to be prepared by the titanium oxide compounding system; The titanium oxide of its weight 2.5 ‰, by 1.5 ‰ phenylformic acid and 0.3 ‰ 2 of phenylformic acid dispenser preparation; 2,6,6-tetramethyl--4-amino piperidine, 0.4 ‰ 3-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid, 0.4 ‰ 3-diethylammonium propylamine and 0.4 ‰ pairs of (2, the 4-di-tert-butyl-phenyl) pentaerythritol diphosphites filter with the standard fine filter.
Claims (2)
1. polymerizing polyamide production technique; The caprolactam fusion; It is characterized in that the fused hexanolactam is with titanium oxide, phenylformic acid, additive charging; After high temperature dynamically mixes, carry out pre-polymerization, post polymerization, extraction in advance, extraction, pelletizing, the dry product that gets, pelletizing, extraction in advance, extraction, drying process are carried out under hermetically sealed system and nitrogen protection
The de-salted water preparation is adopted in the caprolactam fusion, is formulated under the nitrogen-sealed and carries out, and fused hexanolactam and titanium oxide, phenylformic acid, additive filter with the standard fine filter, enter the caprolactam feed system,
The dosage of titanium oxide, phenylformic acid, additive is respectively 2.0-2.5 ‰, 1.2-1.5 ‰, the 1.2-1.5 ‰ of hexanolactam weight,
Said additive is 2,2,6,6-tetramethyl--4-amino piperidine, 3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid, one or more in 3-diethylammonium propylamine and two (2, the 4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
2. adopt the equipment of the polymerization process production polymeric amide of claim 1; Caprolactam fusing system, titanium oxide 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 are arranged, and total system adopts DCS robotization 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 lumped together, and hypomere has the heating coil subassembly;
Extraction tower has steam companions outward, in section extraction sparger is arranged, cat head has header tank; Under annulus inlet distribution device is arranged; Annulus inlet distribution device bottom is taper, and section extraction sparger is a plurality of synergetic awl buckets, and the awl bucket constitutes by falling trapezoidal cone and right circular cone; The space is left in the centre, and falling uniform distribution aperture, trapezoidal cone top is the 8-20mm macropore;
Drying tower has the awl bucket up and down; Awl bucket constitutes by falling trapezoidal cone and right circular cone; Fall and leave the space in the middle of trapezoidal cone and the right circular cone, the water conservancy diversion venting hole is arranged at the right circular cone top, water conservancy diversion venting hole aperture 40-80mm; Falling has the nitrogen air supplying ring that is communicated with the nitrogen blast inlet between trapezoidal cone and top cylindrical shell, bottom cylindrical shell, and 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 whisking appliance, top to be provided with bubble-cap, the heating semicanal arranged outward, in spiral heater is arranged;
Extraction tower top is provided with the blanking conduit in advance, and the bottom is provided with preparatory collection dope charging distributing slot; The riser of extraction tower connects the extraction water recovery system in advance;
On the header tank top of extraction tower cat head section, water separator are arranged, section water sepn net is arranged in section, the water separator, section, water separator are communicated with header tank; The riser of extraction tower connects the extraction water recovery system;
Drying tower bottom cylindrical shell is provided with the section water cooler, and the section water cooler meets the conveying and packaging system.
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| CN103030802A (en) * | 2012-12-20 | 2013-04-10 | 山东华乐新材料科技股份有限公司 | Method for producing semi-dull high-speed spinning domestic section by polymerizing caprolactam |
| CN103289081A (en) * | 2013-06-04 | 2013-09-11 | 武汉森大科技研究发展中心 | Polyamide polymerization production process and equipment for same |
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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 |
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| CN103289081A (en) * | 2013-06-04 | 2013-09-11 | 武汉森大科技研究发展中心 | Polyamide polymerization production process and equipment for same |
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| CN104629041B (en) * | 2015-02-03 | 2016-05-25 | 武汉森大科技研究发展中心 | Nylon-6 continuous polymerization melt vacuum takes off single production technology and equipments |
| CN105801842A (en) * | 2016-04-20 | 2016-07-27 | 温州邦鹿化工有限公司 | Polyamide polymerization production technology |
| CN105801841A (en) * | 2016-04-20 | 2016-07-27 | 温州邦鹿化工有限公司 | Nylon 6 production process and system |
| 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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