CN102796368A - Preparation method of semi-aromatic polyamide alloy - Google Patents
Preparation method of semi-aromatic polyamide alloy Download PDFInfo
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- CN102796368A CN102796368A CN2012102596157A CN201210259615A CN102796368A CN 102796368 A CN102796368 A CN 102796368A CN 2012102596157 A CN2012102596157 A CN 2012102596157A CN 201210259615 A CN201210259615 A CN 201210259615A CN 102796368 A CN102796368 A CN 102796368A
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Abstract
The invention discloses a preparation method of a semi-aromatic polyamide alloy, which is characterized by comprising the steps of: adding 1000-5000 parts by weight of semi-aromatic polyamide prepolymer, 1-50 parts by weight of catalyst, 50-50000 parts by weight of polymer and 1-10 parts by weight of molecular weight modifier into a reaction extruder; reacting and extruding under the conditions that temperature is 280-330 DEG C, screw rotating speed is 20-200rpm and vacuum degree is 0.04-0.09 MPa; and drawing, cooling and chopping the extruded material to obtain the semi-aromatic polyamide alloy.
Description
Technical field
The present invention relates to a kind of preparation method of semi-aromatic polyamide alloy, belong to technical field of polymer materials.
Background technology
Semi-aromatic polyamide is one type of heat-resisting, corrosion resistant macromolecular material, is widely used in fields such as automotive industry, electronic apparatus and daily heat-resisting articles for use.As gather hexamethylene terephthalamide (PA6T) and gather the junctor that paraphenylene terephthalamide's nonamethylene diamine (PA9T) replacement nylon 66 is used to make electron device, can the withstand high temperatures Pb-free solder.Along with development of science and technology, people are also increasingly high to the requirement of material, and it is important that the functionalization of polymkeric substance and high performance also seem all the more.Polymer alloy has the advantage of two or more polymkeric substance concurrently, is a kind of important method of polymers functionization, high performance and cost degradation.
At present the semi-aromatic polyamide alloy mainly adopts virgin resin and modification polymer extruding pelletization to obtain, but the semi-aromatic polyamide synthetic technology of resins is complicated, and resin is synthetic and the blend process in will be through twice granulation, the energy consumption height.Previous work of the present invention openly patent of invention CN102532528A is a raw material with di-carboxylic acid, diamine, nylon salt and amino acid etc.; Elder generation's solid phase polycondensation makes the polymkeric substance of certain molecular weight, extrudes further raising molecular weight through reaction again and obtains the high-molecular weight semi-aromatic polyamide.On this basis, the present invention adopts low-molecular-weight semi-aromatic polyamide performed polymer and modification polymer direct reaction to extrude preparation semi-aromatic polyamide alloy, and this alloy can adopt injection, mold pressing and mode machine-shaping such as extrude.
Summary of the invention
The preparation method who the objective of the invention is to be directed against the deficiency of prior art and a kind of semi-aromatic polyamide alloy is provided; Be characterized in that with the semi-aromatic polyamide performed polymer be raw material; Under the effect of catalyzer and molecular weight regulator; And with the modification polymer blend, preparation semi-aromatic polyamide alloy is extruded in reaction.But this method has operate continuously and the high advantage of yield, and gained semi-aromatic polyamide alloy has the processing of being prone to and the high advantage of mechanical strength.
The object of the invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The preparation method of semi-aromatic polyamide alloy may further comprise the steps:
(1) 1000～5000 parts of semi-aromatic polyamide performed polymers, 1～50 part of catalyzer, 50～50000 parts of modification polymers and molecular weight regulator are added extruder for 1～10 part; Under 280～330 ℃ of temperature, screw speed 20～200rpm and vacuum tightness 0.04～0.09MPa, react and extrude, obtain extrudate;
(2) above-mentioned extrudate is obtained the semi-aromatic polyamide alloy after traction, cooling, pelletizing and drying.
The structural formula of semi-aromatic polyamide performed polymer is:
M=2～20 wherein; 0＜x+y≤1, at least a in x ≠ 0
;
R
1=-(CH
2)
2-,-(CH
2)
4-,-(CH
2)
6-,-(CH
2)
9-with-(CH
2)
10-at least a;
R
2=-(CH
2)
4-and/or-(CH
2)
8-;
R
3=-(CH
2)
5-,-(CH
2)
6-,-(CH
2)
7-,-(CH
2)
8-,-(CH
2)
9-,-(CH
2)
10-with-(CH
2)
11-at least a.
Catalyzer is at least a in phosphoric acid, tetra-sodium, polyphosphoric acid, phosphorous acid, sodium phosphate, Tri sodium Phosphate, sodium phosphite, sodium hypophosphite, propionic acid and the butyric acid.
Modification polymer is polyphenylene sulfide, polyaryl thioether sulfone, polyethersulfone, polysulfones, liquid crystalline polymers, tetrafluoroethylene, perfluoroalkoxy resin, ppe, nylon, gather paraphenylene terephthalamide's glycol ester, gather paraphenylene terephthalamide's butanediol ester, at least a in polycarbonate, PS, Vilaterm, polyolefin elastomer, terpolymer EP rubber and the hydrogenated styrene-butadiene-styrene terpolymer.
Molecular weight regulator is phenylformic acid, p-methylbenzoic acid, m-methyl benzoic acid, o-toluic acid, 1-naphthoic acid, 2-naphthoic acid, LAURIC ACID 99 MIN, Palmiticacid, Triple Pressed Stearic Acid, Tetra hydro Phthalic anhydride or 2, any in the 3-dinicotinic acid acid anhydride.
Performance test:
The semi-aromatic polyamide alloy is injected into the standard batten, adopts Tianjin, the island AGS-J of company type electronic universal material testing machine test mechanical property.
The present invention has following advantage:
1. the method that adopts the reaction of semi-aromatic polyamide performed polymer and modification polymer to extrude is saved the semi-aromatic polyamide synthetic technology of resins, direct production semi-aromatic polyamide alloy.
2. the generation of the adding of modification polymer and semi-aromatic polyamide resin is carried out synchronously, and the interlaminar resin interface junction gets togather, and mechanical strength is high.
3. the kind of semi-aromatic polyamide performed polymer and modification polymer is abundant, can produce multiple semi-aromatic polyamide alloy.
4. the preparation method of semi-aromatic polyamide alloy reacts the weak point that finds time, and has the advantage of energy-conserving and environment-protective.
5. the preparation method of semi-aromatic polyamide alloy, experimental repeatability is good, process stabilizing, product yield is high.
Embodiment
Through embodiment the present invention is carried out concrete description below; Be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; Can not be interpreted as the restriction to the scope of the present invention includes, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
(by terephthalic acid: the weight ratio preparation of hexanodioic acid: hexanediamine=83:73:116) 5000g, phosphoric acid 50g, polyphenylene sulfide 50000g and phenylformic acid 10g add extruder, under 300 ℃ of temperature, screw speed 150rpm and vacuum tightness 0.08MPa, react and extrude with the semi-aromatic polyamide performed polymer; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 94%, tensile strength 81MPa, flexural strength 174MPa, unnotched impact strength 43kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 2
Semi-aromatic polyamide performed polymer (by the weight ratio preparation of terephthalic acid hexanediamine salt: hexanolactam=141:59) 1000g, tetra-sodium 1g, polyaryl thioether sulfone 50g and p-methylbenzoic acid 1g are added extruder, under 320 ℃ of temperature, screw speed 20rpm and vacuum tightness 0.04MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 91%, tensile strength 78MPa, flexural strength 159MPa, unnotched impact strength 36kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 3
With the semi-aromatic polyamide performed polymer (by 4; 4 '-(4-thioether phenylformic acid)-triphenylphosphine oxide: decamethylene diamine: the weight ratio preparation of ring oenantholactam=582:172:46) 3000g, polyphosphoric acid 20g, polyethersulfone 1500g, polysulfones 500g and m-methyl benzoic acid 7g add extruder, under 330 ℃ of temperature, screw speed 200rpm and vacuum tightness 0.09MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 95%, tensile strength 84MPa, flexural strength 165MPa, unnotched impact strength 52kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 4
Semi-aromatic polyamide performed polymer (by the weight ratio preparation of m-phthalic acid ethylenediamine salt: nylon salt=120:180) 1200g, phosphorous acid 10g, nylon 1800g, hydrogenated styrene-butadiene-styrene terpolymer 200g and o-toluic acid 4g are added extruder, under 295 ℃ of temperature, screw speed 80rpm and vacuum tightness 0.07MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 90%, tensile strength 67MPa, flexural strength 137MPa, unnotched impact strength 69kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 5
(by the diphenyl sulfide dimethyl chloride: the weight ratio preparation of sebacoyl chloride: tetramethylenediamine=311:358:220) 2500g, sodium phosphate 15g, liquid crystalline polymers 1000g, tetrafluoroethylene 300g and 1-naphthoic acid 5g add extruder, under 330 ℃ of temperature, screw speed 110rpm and vacuum tightness 0.06MPa, react and extrude with the semi-aromatic polyamide performed polymer; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 95%, tensile strength 96MPa, flexural strength 178MPa, unnotched impact strength 63kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 6
(by the phenyl ether dioctyl phthalate: nonamethylene diamine: the weight ratio preparation of 8-aminocaprylic acid=258:158:84) 3500g, Tri sodium Phosphate 25g, sodium phosphate 15g, perfluoroalkoxy resin 1200g, ppe 500g and 2-naphthoic acid 9g add extruder, under 315 ℃ of temperature, screw speed 140rpm and vacuum tightness 0.09MPa, react and extrude with the semi-aromatic polyamide performed polymer; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 92%, tensile strength 94MPa, flexural strength 182MPa, unnotched impact strength 49kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 7
With the semi-aromatic polyamide performed polymer (by benzophenone dicarboxylic acid: the weight ratio preparation of decamethylene diamine: 9 aminononanoic acid: hexanolactam=270:172:158:50) 3000g, sodium phosphite 35g, gather paraphenylene terephthalamide's glycol ester 1000g, gather paraphenylene terephthalamide's butanediol ester 800g and LAURIC ACID 99 MIN 8g adds extruder, under 290 ℃ of temperature, screw speed 100rpm and vacuum tightness 0.08MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 93%, tensile strength 75MPa, flexural strength 173MPa, unnotched impact strength 54kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 8
(by the sulfobenzide dioctyl phthalate: the weight ratio preparation of the amino capric acid=306:30:53:334 of quadrol: hexanediamine: 10-) 2500g, sodium hypophosphite 20g, polycarbonate 1200g, terpolymer EP rubber 300g and Palmiticacid 6g add extruder, under 285 ℃ of temperature, screw speed 80rpm and vacuum tightness 0.07MPa, react and extrude with the semi-aromatic polyamide performed polymer; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 95%, tensile strength 68MPa, flexural strength 162MPa, unnotched impact strength 66kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 9
With the semi-aromatic polyamide performed polymer (by 4; 4 '-(4-thioether phenylformic acid)-UVNUL MS-40: the weight ratio preparation of the amino hendecoic acid=243:44:163 of tetramethylenediamine: 11-) 4000g, propionic acid 40g, PS 1500g, Vilaterm 500g and Triple Pressed Stearic Acid 10g add extruder, under 280 ℃ of temperature, screw speed 150rpm and vacuum tightness 0.08MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 94%, tensile strength 59MPa, flexural strength 148MPa, unnotched impact strength 52kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 10
With the semi-aromatic polyamide performed polymer (by 4; 4 '-(4-thioether phenylformic acid)-sulfobenzide: 4; 4 '-(4-thioether phenylformic acid)-UVNUL MS-40: the weight ratio preparation of hexanodioic acid: hexanediamine=26:219:146:174) 3800g, butyric acid 45g, polyphenylene sulfide 2000g, polyolefin elastomer 200g and Tetra hydro Phthalic anhydride 10g add extruder, under 310 ℃ of temperature, screw speed 120rpm and vacuum tightness 0.05MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 93%, tensile strength 87MPa, flexural strength 192MPa, unnotched impact strength 56kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 11
With the semi-aromatic polyamide performed polymer by 4; 4 '-(4-oxybenzoic acid)-UVNUL MS-40: the weight ratio preparation of sebacic acid: decamethylene diamine=227:101:172) 3500g, phosphatase 11 5g, polyphosphoric acid 20g, liquid crystalline polymers 1000g and 2; 3-dinicotinic acid acid anhydride 7g adds extruder, under 325 ℃ of temperature, screw speed 180rpm and vacuum tightness 0.09MPa, reacts and extrudes; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 95%, tensile strength 102MPa, flexural strength 207MPa, unnotched impact strength 63kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 12
With the semi-aromatic polyamide performed polymer (by 4; 4 '-(4-oxybenzoic acid)-sulfobenzide: the weight ratio preparation of hexanodioic acid: nonamethylene diamine=245:73:158) 4300g, Tri sodium Phosphate 50g, polyphenylene sulfide 3000g, hydrogenated styrene-butadiene-styrene terpolymer 1200g and o-toluic acid 9g add extruder, under 300 ℃ of temperature, screw speed 170rpm and vacuum tightness 0.07MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 92%, tensile strength 86MPa, flexural strength 188MPa, unnotched impact strength 71kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 13
(by the triphenylphosphine oxide dioctyl phthalate: the weight ratio preparation of decamethylene diamine: hexanolactam=183:86:81) 4000g, phosphorous acid 40g, polyaryl thioether sulfone 1500g and 2-naphthoic acid 10g add extruder, under 325 ℃ of temperature, screw speed 140rpm and vacuum tightness 0.06MPa, react and extrude with the semi-aromatic polyamide performed polymer; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 94%, tensile strength 73MPa, flexural strength 179MPa, unnotched impact strength 64kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 14
With the semi-aromatic polyamide performed polymer (by 4; 4 '-(4-oxybenzoic acid)-triphenylphosphine oxide: tetramethylenediamine: the weight ratio preparation of ring oenantholactam=275:44:171) 3300g, propionic acid 5g, phosphoric acid 25g, nylon 2000g and phenylformic acid 7g add extruder, under 290 ℃ of temperature, screw speed 90rpm and vacuum tightness 0.08MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 95%, tensile strength 76MPa, flexural strength 173MPa, unnotched impact strength 49kJ/m after traction, cooling, pelletizing and drying
2
Embodiment 15
With the semi-aromatic polyamide performed polymer (by terephthalic acid hexanediamine salt: the weight ratio preparation of nylon salt: hexanolactam=846:524:113) 2700g, sodium phosphite 40g, gather paraphenylene terephthalamide's butanediol ester 2300g and Triple Pressed Stearic Acid 6g adds extruder, under 300 ℃ of temperature, screw speed 130rpm and vacuum tightness 0.07MPa, react and extrude; Extrudate obtains the semi-aromatic polyamide alloy, productive rate 93%, tensile strength 81MPa, flexural strength 167MPa, unnotched impact strength 53kJ/m after traction, cooling, pelletizing and drying
2
Claims (5)
1. the preparation method of a semi-aromatic polyamide alloy is characterized in that this method may further comprise the steps:
(1) by weight; 1000～5000 parts of semi-aromatic polyamide performed polymers, 1～50 part of catalyzer, 50～50000 parts of modification polymers and molecular weight regulator are added extruder for 1～10 part; Under 280～330 ℃ of temperature, screw speed 20～200rpm and vacuum tightness 0.04～0.09MPa, react and extrude, obtain extrudate;
(2) above-mentioned extrudate is obtained the semi-aromatic polyamide alloy after traction, cooling, pelletizing and drying.
2. according to the preparation method of the said semi-aromatic polyamide alloy of claim 1, it is characterized in that the structural formula of semi-aromatic polyamide performed polymer is:
M=2～20 wherein; 0＜x+y≤1, at least a in x ≠ 0
;
R
1=-(CH
2)
2-,-(CH
2)
4-,-(CH
2)
6-,-(CH
2)
9-with-(CH
2)
10-at least a;
R
2=-(CH
2)
4-and/or-(CH
2)
8-;
R
3=-(CH
2)
5-,-(CH
2)
6-,-(CH
2)
7-,-(CH
2)
8-,-(CH
2)
9-,-(CH
2)
10-with-(CH
2)
11-at least a.
3. according to the preparation method of the said semi-aromatic polyamide alloy of claim 1, it is characterized in that catalyzer is at least a in phosphoric acid, tetra-sodium, polyphosphoric acid, phosphorous acid, sodium phosphate, Tri sodium Phosphate, sodium phosphite, sodium hypophosphite, propionic acid and the butyric acid.
4. according to the preparation method of the said semi-aromatic polyamide alloy of claim 1, it is characterized in that modification polymer be polyphenylene sulfide, polyaryl thioether sulfone, polyethersulfone, polysulfones, liquid crystalline polymers, tetrafluoroethylene, perfluoroalkoxy resin, ppe, nylon, gather paraphenylene terephthalamide's glycol ester, gather paraphenylene terephthalamide's butanediol ester, at least a in polycarbonate, PS, Vilaterm, polyolefin elastomer, terpolymer EP rubber and the hydrogenated styrene-butadiene-styrene terpolymer.
5. according to the preparation method of the said semi-aromatic polyamide alloy of claim 1; It is characterized in that molecular weight regulator is phenylformic acid, p-methylbenzoic acid, m-methyl benzoic acid, o-toluic acid, 1-naphthoic acid, 2-naphthoic acid, LAURIC ACID 99 MIN, Palmiticacid, Triple Pressed Stearic Acid, Tetra hydro Phthalic anhydride or 2, any in the 3-dinicotinic acid acid anhydride.
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| CN110156985A (en) * | 2019-04-30 | 2019-08-23 | 珠海派锐尔新材料有限公司 | A kind of high fluidity random copolymerization semi-aromatic nylon and preparation method thereof |
| CN111471298A (en) * | 2020-04-22 | 2020-07-31 | 建湖县兴隆尼龙有限公司 | Toughened nylon material and preparation method thereof |
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