CN105820331A - Polyamide polymerization production process - Google Patents

Polyamide polymerization production process Download PDF

Info

Publication number
CN105820331A
CN105820331A CN201610245760.8A CN201610245760A CN105820331A CN 105820331 A CN105820331 A CN 105820331A CN 201610245760 A CN201610245760 A CN 201610245760A CN 105820331 A CN105820331 A CN 105820331A
Authority
CN
China
Prior art keywords
dried
caprolactam
polymerization
nitrogen
titanium dioxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610245760.8A
Other languages
Chinese (zh)
Inventor
许道沈
林洁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wenzhou Banglu Chemical Co Ltd
Original Assignee
Wenzhou Banglu Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wenzhou Banglu Chemical Co Ltd filed Critical Wenzhou Banglu Chemical Co Ltd
Priority to CN201610245760.8A priority Critical patent/CN105820331A/en
Publication of CN105820331A publication Critical patent/CN105820331A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/08Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
    • C08G69/14Lactams
    • C08G69/16Preparatory processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/08Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
    • C08G69/14Lactams
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyamides (AREA)

Abstract

The invention discloses a polyamide polymerization production process. As monobasic acid is taken as a chemical reaction chain terminator, together with added SEED and benzylamine, the problems that in the prior art titanium dioxide can be precipitated and scale can be caused when binary acid as the chemical reaction chain terminator is mixed with titanium dioxide and SEED are solved, and moreover, the rheological property, the thermal stability, the dyeing property and the thermal stability of polyamide 6 can be improved.

Description

A kind of polymerizing polyamide production technology
Technical field
The present invention relates to chemical products field, be specifically related to a kind of polymerizing polyamide production technology.
Background technology
At present China mainly quotes import equipment and external advanced technologies for polyamide silk floss synthetic fibre 6 polymerization technique of cutting into slices, and it mainly has Ji Ma, Yi Wenda mono-card Fischer, A Jiafei, noy etc..And the equipment introduced and technique are all had no idea for high-end civilian high-speed spinning section, will become apparent from particular for high-end fine-denier spinning section problem, the section produced is only used for producing conventional section and low side engineering plastics are cut into slices, thus causes and domestic be the most also dependent on import for high-end civilian section.Import equipment is made up of caprolactam melting device, titanium dioxide dispenser, benzoic acid distributor, caprolactam feed column, pre-polymerization tower, post polymerization tower, granulating device, extraction tower, drying tower and conveying and packaging part, and whole system uses DCS Automated condtrol.Polymerizing polyamide production technology is that melted caprolactam feeds together with titanium dioxide, benzoic acid, through pre-polymerization, post polymerization, pelletizing, extract, be dried to obtain product.
And in existing amide polymerization technique, owing to titanium dioxide plays photoextinction in polymerizing polyamide, and titanium dioxide can make under titanium dioxide precipitation with binary acid and SEED mix process, so will result in titanium dioxide and form shell in the tubulation of pre-polymerization pipe, make production reaction to go on normally.
Summary of the invention
In order to solve the shortcoming of prior art, the present invention provides a kind of polymerizing polyamide production technology.
The technical solution that the present invention uses is: a kind of polymerizing polyamide production technology; in parts by weight; caprolactam is melted; use nitrogen-sealed; desalted water is used to prepare; melted caprolactam and the monoacid of 0.1-0.6%; the SEED of 0.05-0.4%; the benzylamine of 0-0.4%, the titanium dioxide of 0-1.5%, with twice filtration of fine filter; enter caprolactam feed system; through pre-polymerization, post polymerization, pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.
A kind of polymerizing polyamide production technology, in parts by weight, melts caprolactam; use nitrogen-sealed, use desalted water to prepare, melted caprolactam and the monoacid of 0.1-0.4%; the SEED of 0.1-0.3%; the benzylamine of 0-0.2%, the titanium dioxide of 0-1.5%, with twice filtration of fine filter; enter caprolactam feed system; through pre-polymerization, post polymerization, pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.
Described monoacid is benzoic acid or acetic acid.
Described is dried as continuous drying, and being dried is to seal to be dried under nitrogen circulation, temperature 110-145 ° C, 12-34 hour time.
The invention has the beneficial effects as follows: a kind of polymerizing polyamide production technology, by using monoacid as chemical reaction chain terminating agent, coordinate the SEED and benzylamine added, solve in prior art binary acid chemistry as reaction chain terminator with titanium dioxide and SEED are during mixing under titanium dioxide precipitation, the problem of fouling, and improve the rheological characteristic of polyamide 6, heat stability and dyeability and heat stability.
Detailed description of the invention
Embodiment 1
A kind of polymerizing polyamide production technology, in parts by weight, caprolactam is melted, use nitrogen-sealed, desalination circulation soft water and chilled water is used to prepare, melted caprolactam and the benzoic acid of 0.1%, the SEED of 0.4%, benzylamine: 0.2%, titanium dioxide: 1.5% uses twice filtration of fine filter, enter caprolactam feed system, through pre-polymerization, post polymerization, pelletizing, extraction, it is dried and finally gives product, it is dried and carries out under Full-closed system and nitrogen are protected, drying steps is continuous drying, described is predrying, dry run is carried out under Full-closed system and nitrogen are protected, 110 ° of C of described baking temperature, 12 hours time.
Embodiment 2
A kind of polymerizing polyamide production technology; in parts by weight; caprolactam is melted; use nitrogen-sealed; desalination circulation soft water and chilled water is used to prepare; melted caprolactam and the benzoic acid of 0.6%, the SEED of 0.05%, benzylamine: 0.4%; titanium dioxide: 1% uses twice filtration of fine filter; enter caprolactam feed system, through pre-polymerization, post polymerization, pelletizing, extract, be dried and finally give product; it is dried and carries out under Full-closed system and nitrogen are protected; drying steps is continuous drying, 125 ° of C of baking temperature, 20 hours time.
Embodiment 3
A kind of polymerizing polyamide production technology, in parts by weight, melts caprolactam; use nitrogen-sealed; desalination circulation soft water and chilled water is used to prepare, melted caprolactam and the acetic acid of 0.4%, the SEED of 0.3%; benzylamine: 0.2%; titanium dioxide: 1.5%, with twice filtration of fine filter, enters caprolactam feed system, through pre-polymerization, post polymerization; pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.Drying steps is 130 ° of C of continuous drying, described baking temperature, 30 hours time.
Embodiment 4
A kind of polymerizing polyamide production technology, in parts by weight, melts caprolactam; use nitrogen-sealed; desalination circulation soft water and chilled water is used to prepare, melted caprolactam and the acetic acid of 0.1%, the SEED of 0.2%; benzylamine: 0.2%; titanium dioxide: 1.5%, with twice filtration of fine filter, enters caprolactam feed system, through pre-polymerization, post polymerization; pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.Drying steps is 145 ° of C of continuous drying, described baking temperature, 34 hours time.
The present invention solves in existing polymerizing polyamide production technology, titanium dioxide can make under titanium dioxide precipitation with binary acid and SEED mix process, so will result in titanium dioxide and form shell in the tubulation of pre-polymerization pipe, making production reaction to go on normally, the present invention with the addition of SEED and improves polyamide 6 rheological characteristic, heat stability and dyeability;Add the improvement polyamide 6 dyeability of benzylamine, heat stability.Use monoacid as unique chemical reaction chain terminating agent, solve titanium dioxide forms shell fouling in polyamide polymerization process problem in the tubulation of pre-polymerization pipe.

Claims (4)

1. a polymerizing polyamide production technology, it is characterised in that in parts by weight; caprolactam is melted, uses nitrogen-sealed, use desalted water to prepare; melted caprolactam and the monoacid of 0.1-0.6%, the benzylamine of the SEED of 0.05-0.4%, 0-0.4%; the titanium dioxide of 0-1.5%; with twice filtration of fine filter, enter caprolactam feed system, through pre-polymerization, post polymerization; pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.
A kind of polymerizing polyamide production technology the most according to claim 1; it is characterized in that; in parts by weight; caprolactam is melted; use nitrogen-sealed; desalted water is used to prepare; melted caprolactam and the monoacid of 0.1-0.4%; the SEED of 0.1-0.3%, benzylamine: 0-0.2%, titanium dioxide: 0-1.5% twice filtration of fine filter; enter caprolactam feed system; through pre-polymerization, post polymerization, pelletizing, extract, be dried and finally give product, be dried and carry out under Full-closed system and nitrogen are protected.
A kind of polymerizing polyamide production technology the most according to claim 1, it is characterised in that described monoacid is benzoic acid or acetic acid.
A kind of polymerizing polyamide production technology the most according to claim 1, it is characterised in that described is dried as continuous drying, being dried is to seal to be dried under nitrogen circulation, temperature 110-145 ° C, 12-34 hour time.
CN201610245760.8A 2016-04-20 2016-04-20 Polyamide polymerization production process Pending CN105820331A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610245760.8A CN105820331A (en) 2016-04-20 2016-04-20 Polyamide polymerization production process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610245760.8A CN105820331A (en) 2016-04-20 2016-04-20 Polyamide polymerization production process

Publications (1)

Publication Number Publication Date
CN105820331A true CN105820331A (en) 2016-08-03

Family

ID=56526181

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610245760.8A Pending CN105820331A (en) 2016-04-20 2016-04-20 Polyamide polymerization production process

Country Status (1)

Country Link
CN (1) CN105820331A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108948344A (en) * 2017-05-19 2018-12-07 江苏永通新材料科技有限公司 Polycaprolactam auxiliary agent and preparation method thereof, polycaprolactam
WO2022042565A1 (en) * 2020-08-31 2022-03-03 聊城鲁西聚酰胺新材料科技有限公司 Nylon 6 production process, system, and product

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR970021133A (en) * 1995-10-19 1997-05-28 이웅렬 Method for producing polyamide having excellent titanium dioxide dispersibility
KR20030012336A (en) * 2001-07-31 2003-02-12 주식회사 효성 The Manufacturing Method Of Polyamide Polymer Having Superior Dispersibility For Titanium Dioxide
KR20030034845A (en) * 2001-10-29 2003-05-09 주식회사 효성 The manufacturing method of polyamid with a good dispersing of titanium dioxide
CN1714179A (en) * 2002-11-22 2005-12-28 可隆株式会社 A full dull polyamide 6 yarn, and a process of preparing for the same
CN101050279A (en) * 2007-05-09 2007-10-10 武汉森大科技研究发展中心 Production technique and equipment for polymerizing polyamide
CN201301295Y (en) * 2008-07-10 2009-09-02 广东新会美达锦纶股份有限公司 Stirrer device used for full-dull chinlon 6 polymerization pipe
CN101880386A (en) * 2010-07-09 2010-11-10 北京三联虹普纺织化工技术有限公司 Recovery method of hexanolactam in polyamide-6 continuous polymerization production process
CN102775600A (en) * 2012-08-01 2012-11-14 武汉森大科技研究发展中心 Polymerization manufacturing technique and device for polyamide
CN103159951A (en) * 2011-12-13 2013-06-19 上海杰事杰新材料(集团)股份有限公司 Method and apparatus for preparing high temperature nylon
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
CN103408749A (en) * 2013-07-09 2013-11-27 江苏海阳化纤有限公司 Chinlon 6 section for bromochlorodifluoromethane (BCF) carpet yarn and preparation method thereof

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR970021133A (en) * 1995-10-19 1997-05-28 이웅렬 Method for producing polyamide having excellent titanium dioxide dispersibility
KR20030012336A (en) * 2001-07-31 2003-02-12 주식회사 효성 The Manufacturing Method Of Polyamide Polymer Having Superior Dispersibility For Titanium Dioxide
KR20030034845A (en) * 2001-10-29 2003-05-09 주식회사 효성 The manufacturing method of polyamid with a good dispersing of titanium dioxide
CN1714179A (en) * 2002-11-22 2005-12-28 可隆株式会社 A full dull polyamide 6 yarn, and a process of preparing for the same
CN101050279A (en) * 2007-05-09 2007-10-10 武汉森大科技研究发展中心 Production technique and equipment for polymerizing polyamide
CN201301295Y (en) * 2008-07-10 2009-09-02 广东新会美达锦纶股份有限公司 Stirrer device used for full-dull chinlon 6 polymerization pipe
CN101880386A (en) * 2010-07-09 2010-11-10 北京三联虹普纺织化工技术有限公司 Recovery method of hexanolactam in polyamide-6 continuous polymerization production process
CN103159951A (en) * 2011-12-13 2013-06-19 上海杰事杰新材料(集团)股份有限公司 Method and apparatus for preparing high temperature nylon
CN102775600A (en) * 2012-08-01 2012-11-14 武汉森大科技研究发展中心 Polymerization manufacturing technique and device for polyamide
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
CN103408749A (en) * 2013-07-09 2013-11-27 江苏海阳化纤有限公司 Chinlon 6 section for bromochlorodifluoromethane (BCF) carpet yarn and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王琛: "《高分子材料改性技术》", 30 April 2007, 中国纺织出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108948344A (en) * 2017-05-19 2018-12-07 江苏永通新材料科技有限公司 Polycaprolactam auxiliary agent and preparation method thereof, polycaprolactam
WO2022042565A1 (en) * 2020-08-31 2022-03-03 聊城鲁西聚酰胺新材料科技有限公司 Nylon 6 production process, system, and product

Similar Documents

Publication Publication Date Title
CN103289081B (en) Polymerizing polyamide production technique and equipment used
CN102070127B (en) Method for producing insoluble sulfur
CN108660524B (en) Sea-island fiber composite melt spinning method using water-soluble modified PVA as sea
CN102382296A (en) Production process for preparing fiber-grade nylon 6 chips with extracted aqueous concentrated solution and apparatus thereof
CN105820331A (en) Polyamide polymerization production process
CN102775600A (en) Polymerization manufacturing technique and device for polyamide
CN109679339A (en) A kind of improvement release property and 56 composition of polyamide flexible and its application
JP6025829B2 (en) Method and apparatus for direct, continuous modification of polymer melts
CN103304788B (en) Preparation method of polybutylene terephthalate polyester resin
WO2007035251A3 (en) Late addition to effect compositional modifications in condensation polymers
CN100509917C (en) Polyamide prepolymer, polyamide ,and processes for producing these
CN104072755A (en) Novel three kettle polymerization process of chinlon 6
CN104098772A (en) Novel polyamide-imide preparation method
CN107417907A (en) A kind of preparation method of high crystalline poly (arylene ether nitrile)
CN105801842A (en) Polyamide polymerization production technology
ID29347A (en) PROCESS AND APARATUS FOR PRODUCING GRANUL, SPECIALLY GRANUL PET, FROM POLIFUNCTIONAL AND ALCOHOL CARBOXICATE ACID
CN108570147A (en) A kind of 6 coloured slice continuous production device of polyamide fibre and production method
CN105801841A (en) Nylon 6 production process and system
CN206318923U (en) Chinlon 6 section continuous polymerization process units
CN207998575U (en) A kind of 6 coloured slice continuous production device of polyamide fibre
CN203295414U (en) Polyamide polymerization production equipment
CN101280472B (en) Special-shaped monofilament section and production method thereof
CN207930911U (en) A kind of 6 black of polyamide fibre slice continuous production device
CN100395387C (en) Method for preparing polyacrylonitrile pomace
CN206318922U (en) Caprolactam polymerization extraction concentrate reuse manufacture chinlon 6 section process units

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160803

RJ01 Rejection of invention patent application after publication