CN104530421A - Semi-aromatic polyamide preparation method - Google Patents
Semi-aromatic polyamide preparation method Download PDFInfo
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- CN104530421A CN104530421A CN201510002221.7A CN201510002221A CN104530421A CN 104530421 A CN104530421 A CN 104530421A CN 201510002221 A CN201510002221 A CN 201510002221A CN 104530421 A CN104530421 A CN 104530421A
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- pa10t
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- decamethylene diamine
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- paraphenylene terephthalamide
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Abstract
The invention relates to a semi-aromatic polyamide preparation method. The method comprises the steps that decamethylene diamine and terephthalic acid are used as main raw materials, a small amount of water is used as a solvent for preparing a semi-aromatic polyamide salt, a semi-aromatic polyamide preformed polymer is obtained after high temperature and high pressure are kept for a short time, and finally semi-aromatic polyamide is obtained through solid-phase viscosity increasing or fusion viscosity increasing. The method has the advantages that the salt is made by using water as the solvent, the water consumption amount is small, the polymerization process is short, the requirement for equipment is not high by the adoption of conventional equipment, and continuous production is facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of polymeric amide, especially a kind of preparation method of semiaromatic polyamide composition.
Background technology
Semiaromatic polyamide composition is the polymeric amide being with the diamines of aromatic ring or dicarboxylic acid to prepare with aliphatic dicarboxylic acid or diamines polycondensation.Owing to having imported aromatic ring in polyamide molecule main chain, semiaromatic polyamide composition has had higher thermotolerance and water-intake rate than conventional polymeric amide (as nylon 6, nylon66 fiber).Along with developing rapidly of technology, electron trade and car industry have higher requirement to performances such as the thermotolerances of used polymeric amide, and this makes semiaromatic polyamide composition have broad application prospects in these areas.
When synthetic nylon, for the ease of controlling the molar ratio of diprotic acid, diamine, and remove the impurity in monomer, the method that nylon salt carries out polycondensation is more first made in usual employing.Patent CN101456804 discloses a kind of organism that adopts as the semi-aromatic nylon salt preparation method of solvent, but relative to use water as solvent, comparatively large with organic solvent cost, and have the hidden danger of secure context.Patent CN 1887841 discloses a kind of method preparing semi-aromatic nylon salt using water as solvent, but the method water consumption is comparatively large, and production efficiency is difficult to improve.
Patent US5516882, US5981692 and US962628 describe with to benzene first diacid, m-phthalic acid, 1,6-hexanodioic acid, 1,6-hexanediamine and 2-methyl isophthalic acid, 5-pentamethylene diamine is main raw material, is carried out the method for synthesizing polyamides 6T multipolymer by the high-temperature fusion polymerizations of more than 300 DEG C.Patent US6140459 to describe with terephthalic acid, 1,6-hexanediamine and another kind of aliphatic long-chain di-carboxylic acid as raw material, carrys out synthesizing polyamides 6T multipolymer by melt polymerization.When adopting melt polymerization to prepare semiaromatic polyamide composition, secondary polymerization reaction temperature can exceed the fusing point of polymkeric substance, and at high temperature overstand, the DeR of various side reaction and polymkeric substance is violent, easily causes the phenomenon that polymkeric substance tone is deteriorated, physical strength reduces and formability degenerates.Patent US615869 describes first to be had under water existent condition, synthesizes low limiting viscosity prepolymer, then prepares the method for polyamide 9T through solid-phase tack producing reaction.The problem of the method is to obtain the higher prepolymer of limiting viscosity, needs to keep prepolymer to be liquid state, needs to add more water, cause reaction pressure to improve like this in pre-polymerization process, also wants corresponding raising to the requirement of equipment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of preparation method of semiaromatic polyamide composition, the method water consumption is less, and polymerization process flow process is short, less demanding to equipment, is convenient to continuous prodution.
According to technical scheme provided by the invention, a kind of preparation method of semiaromatic polyamide composition, is characterized in that, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 45-55 part, terephthalic acid 45-55 part, oxidation inhibitor 0.1-0.5 part, molecular weight regulator 0.01-0.2 part and catalyzer 0.1-0.5 part, at temperature 140-160 DEG C, react after 0.5-1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (i.e. PA10T) salts solution, then sampling and measuring acidity, acidity control is at 0.1-2;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 25-80 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 80-120 DEG C, and time of drying is 1-2 hour, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 300-320 DEG C, the residence time is 8-10 minute, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is put into solid-phase tack producing still and carry out thickening, thickening temperature is 200-280 DEG C, and the thickening time is 10-40 hour; Or PA10T performed polymer is sent into the extrusion equipment with venting port, under the condition vacuumized, carry out melting thickening, thickening temperature is 320-350 DEG C, and the residence time is 1-8 minute, and vacuum tightness is-0.1 ~-0.09MPa, obtains PA10T resin.
Described molecular weight regulator is phenylformic acid, acetic acid or propionic acid.
Described catalyzer is phosphorous acid, sodium hypophosphite or sodium phosphite.
The present invention with decamethylene diamine, terephthalic acid for main raw material, make solvent with less water and prepare semiaromatic polyamide composition salt, semiaromatic polyamide composition performed polymer is prepared through short time high temperature high pressure, obtain semiaromatic polyamide composition finally by solid-phase tack producing or melting thickening, the advantage of the method is that making salt uses water as solvent, and water consumption is less, polymerization process flow process is short, adopt conventional equipment, less demanding to equipment, be convenient to continuous prodution.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Oxidation inhibitor of the present invention can select commercial goods as oxidation inhibitor P-EPQ, oxidation inhibitor 1098, irgasfos 168, antioxidant 1010 or antioxidant 1076; Described molecular weight regulator is phenylformic acid, acetic acid or propionic acid; Described catalyzer is phosphorous acid, sodium hypophosphite or sodium phosphite.
Embodiment 1
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 51 parts, terephthalic acid 49 parts, oxidation inhibitor P-EPQ 0.1 part, 0.01 part, phenylformic acid and 0.1 part, phosphorous acid, at temperature 140 DEG C, react after 1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 0.1-0.6;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 25 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 100 DEG C, and time of drying is 1 hour, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 300 DEG C, the residence time is 10 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is put into solid-phase tack producing still and carry out thickening, thickening temperature is 200 DEG C, and the thickening time is 40 hours, obtains PA10T resin.
Embodiment 2
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 45 parts, terephthalic acid 55 parts, irgasfos 168 0.1 part, acetic acid 0.1 part and sodium hypophosphite 0.3 part, at temperature 150 DEG C, react after 1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 0.7-1;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 50 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 120 DEG C, and time of drying is 1.5 hours, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 310 DEG C, the residence time is 9 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is put into solid-phase tack producing still and carry out thickening, thickening temperature is 240 DEG C, and the thickening time is 20 hours, obtains PA10T resin.
Embodiment 3
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 55 parts, terephthalic acid 45 parts, antioxidant 1076 0.5 part, propionic acid 0.2 part and sodium phosphite 0.5 part, at temperature 160 DEG C, react after 0.5 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 1-2;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 80 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 80 DEG C, and time of drying is 2 hours, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 320 DEG C, the residence time is 8 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is put into solid-phase tack producing still and carry out thickening, thickening temperature is 280 DEG C, and the thickening time is 10 hours, obtains PA10T resin.
Embodiment 4
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 51 parts, terephthalic acid 49 parts, oxidation inhibitor P-EPQ 0.1 part, 0.01 part, phenylformic acid and 0.1 part, phosphorous acid, at temperature 140 DEG C, react after 1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 0.1-0.6;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 25 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 100 DEG C, and time of drying is 1 hour, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 300 DEG C, the residence time is 10 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is sent into the extrusion equipment with venting port, under the condition vacuumized, carry out melting thickening, thickening temperature is 320 DEG C, and the residence time is 8 minutes, and vacuum tightness is 300Pa, obtains PA10T resin.
Embodiment 5
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 51 parts, terephthalic acid 49 parts, irgasfos 168 0.1 part, acetic acid 0.1 part and sodium hypophosphite 0.3 part, at temperature 150 DEG C, react after 1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 0.7-1;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 50 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 100 DEG C, and time of drying is 1.5 hours, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 310 DEG C, the residence time is 9 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is sent into the extrusion equipment with venting port, under the condition vacuumized, carry out melting thickening, thickening temperature is 340 DEG C, and the residence time is 5 minutes, and vacuum tightness is 100Pa, obtains PA10T resin.
Embodiment 6
The preparation method of semiaromatic polyamide composition, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 51 parts, terephthalic acid 49 parts, antioxidant 1076 0.5 part, propionic acid 0.2 part and sodium phosphite 0.5 part, at temperature 160 DEG C, react after 0.5 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine (PA10T) salts solution, then sampling and measuring acidity, acidity control is at 1-2;
(2) by the crystallization in a crystallizer of PA10T salts solution, Tc is 80 DEG C, obtains PA10T salt-pepper noise;
(3) PA10T salt-pepper noise is put into whizzer, dry, obtain wet PA10T salt;
(4) wet PA10T salt is put into dry pot dry, drying temperature is 100 DEG C, and time of drying is 2 hours, obtains dry PA10T salt;
(5) dry PA10T salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 320 DEG C, the residence time is 8 minutes, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain PA10T performed polymer;
(6) PA10T performed polymer is sent into the extrusion equipment with venting port, under the condition vacuumized, carry out melting thickening, thickening temperature is 350 DEG C, and the residence time is 1 minute, and vacuum tightness is 50Pa, obtains PA10T resin.
Claims (3)
1. a preparation method for semiaromatic polyamide composition, is characterized in that, comprises the following steps:
(1) dropping into material to making in salt oven, counting by weight:
100 parts, water, decamethylene diamine 45-55 part, terephthalic acid 45-55 part, oxidation inhibitor 0.1-0.5 part, molecular weight regulator 0.01-0.2 part and catalyzer 0.1-0.5 part, at temperature 140-160 DEG C, react after 0.5-1 hour and obtain poly-paraphenylene terephthalamide's decamethylene diamine salts solution, then sampling and measuring acidity, acidity control is at 0.1-2;
(2) will gather the crystallization in a crystallizer of paraphenylene terephthalamide's decamethylene diamine salts solution, Tc is 25-80 DEG C, obtains PA10T salt-pepper noise;
(3) poly-paraphenylene terephthalamide's decamethylene diamine salt-pepper noise is put into whizzer, dry, obtain wet poly-paraphenylene terephthalamide's decamethylene diamine salt;
(4) wet poly-paraphenylene terephthalamide's decamethylene diamine salt is put into dry pot dry, drying temperature is 80-120 DEG C, and time of drying is 1-2 hour, obtains dry poly-paraphenylene terephthalamide's decamethylene diamine salt;
(5) dry poly-paraphenylene terephthalamide's decamethylene diamine salt is sent into twin screw extruder by continuous feeding device, the temperature of twin screw extruder is 300-320 DEG C, the residence time is 8-10 minute, obtain PA10T performed polymer melt, PA10T performed polymer melt is by being arranged on the nozzle ejection of twin screw extruder end, reclaim in the form of a powder, obtain poly-paraphenylene terephthalamide's decamethylene diamine performed polymer;
(6) poly-paraphenylene terephthalamide's decamethylene diamine performed polymer is put into solid-phase tack producing still and carry out thickening, thickening temperature is 200-280 DEG C, and the thickening time is 10-40 hour; Or PA10T performed polymer is sent into the extrusion equipment with venting port, under the condition vacuumized, carry out melting thickening, thickening temperature is 320-350 DEG C, and the residence time is 1-8 minute, and vacuum tightness is-0.1 ~-0.09MPa, obtains PA10T resin.
2. the preparation method of semi-aromatic nylon as claimed in claim 1, is characterized in that: described molecular weight regulator is phenylformic acid, acetic acid or propionic acid.
3. the preparation method of semi-aromatic nylon as claimed in claim 1, is characterized in that: described catalyzer is phosphorous acid, sodium hypophosphite or sodium phosphite.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106700064A (en) * | 2016-12-28 | 2017-05-24 | 浙江新和成特种材料有限公司 | Semi-aromatic polyamide production method and semi-aromatic polyamide |
CN109467694A (en) * | 2018-10-12 | 2019-03-15 | 广州市万佳成塑料有限公司 | A kind of production method of low molecular weight nylon 9 T powder synthesis high molecular weight nylon 9T resin |
WO2019137303A1 (en) * | 2018-01-10 | 2019-07-18 | 金发科技股份有限公司 | Polyamide having high crystallization rate, preparation method therefor and application thereof |
CN114316255A (en) * | 2022-01-21 | 2022-04-12 | 湖南世博瑞高分子新材料有限公司 | High-temperature-resistant nylon continuous melt polymerization method |
US11505649B2 (en) | 2017-09-28 | 2022-11-22 | Dupont Polymers, Inc. | Polymerization process |
CN116874771A (en) * | 2023-09-07 | 2023-10-13 | 中国天辰工程有限公司 | Continuous production method of high-temperature nylon powder with narrow molecular weight distribution |
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CN116874771A (en) * | 2023-09-07 | 2023-10-13 | 中国天辰工程有限公司 | Continuous production method of high-temperature nylon powder with narrow molecular weight distribution |
CN116874771B (en) * | 2023-09-07 | 2024-01-23 | 中国天辰工程有限公司 | Continuous production method of high-temperature nylon powder with narrow molecular weight distribution |
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Application publication date: 20150422 |