CN1865351A - Anion in situ preparation method of polysulfone analog/MC nylon6 composite material - Google Patents

Anion in situ preparation method of polysulfone analog/MC nylon6 composite material Download PDF

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Publication number
CN1865351A
CN1865351A CN 200610040169 CN200610040169A CN1865351A CN 1865351 A CN1865351 A CN 1865351A CN 200610040169 CN200610040169 CN 200610040169 CN 200610040169 A CN200610040169 A CN 200610040169A CN 1865351 A CN1865351 A CN 1865351A
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China
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nylon
composite material
anion
polysulfones
vacuum
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CN 200610040169
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CN100516141C (en
Inventor
林志勇
钱浩
陈婉吟
黄丽丹
黄锦河
陈瑜
姚辉梅
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Huaqiao University
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Huaqiao University
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Publication of CN100516141C publication Critical patent/CN100516141C/en
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Abstract

The invention discloses an anion home position preparing method of polysulfone and MC nylon 6 composite material, which comprises the following steps: melting caprolactam monomer; dewatering in the vacuum; adding catalyst to dewater in the vacuum continually; adding polysulfone resin; stirring through magnetism to disperse polysulfone; adding activator; casting the mixture in the preheat mould; demoulding to produce the composite material of polysulfone and MC nylon 6. The invention possesses certain elastic modulus, bending strength, which improves the heat-durability of pure MC nylon by 80 deg.c.

Description

The anion in situ preparation method of polysulfones/MC nylon 6 composite material
Technical field
The present invention relates to adopt anionic polymerization to prepare original position polysulfones/MC nylon 6 composite material, belong to materials science field.
Background technology
Monomer cast nylon 6 (MC nylon 6) is a kind of in the nylon material, its preparation method is with fused hexanolactam decompression dehydration under normal pressure, and add strong alkaline substance and make catalyzer further after the dehydration, be mixed with activator auxiliary agents such as (as isocyanic ester), directly be injected in the mould of preheating certain temperature, material carries out the rapid polymerization reaction in mould, be frozen into solid blank.MC nylon has that polymerization temperature is low, technology is simple, degree of crystallinity is high, molecular weight is big, mechanical property is higher than advantages such as common nylon, abrasion performance, self-lubricating, damping and silencing, grease resistance, in field extensive application such as mechanical component, weaving, petrochemical complex, national defense industry, as large-scale ball valve seal ring and the axle sleeve on oil, the natural gas transmission pipeline, various transfer members such as bearing shell, axle sleeve, weaving loom shuttle, gear etc.Along with further expanding of MC nylon range of application, it is good etc. that its performance has been proposed more and more higher requirement, particularly its dimensional stability and thermostability, is difficult to satisfy the high performance requirement of large parts.Therefore, how to keep improving its heat-resistant stability on the basis of MC nylon very good mechanical properties, become the key of expansion MC nylon range of application.
Summary of the invention
The object of the present invention is to provide the anion in situ preparation method of a kind of polysulfones/MC nylon 6 composite material, the premium properties that not only has MC nylon 6 by the matrix material of this method preparation, and the mechanical property more outstanding than MC nylon 6, particularly resistance toheat is greatly improved.
Technical scheme of the present invention is such, and the anion in situ preparation method of polysulfones/MC nylon 6 composite material is realized through the following steps:
The first step is heated to 100-120 ℃ with caprolactam monomer in reaction vessel, make material melting, vacuum hydro-extraction, and vacuum tightness is 10 -1-10 -3Pa adds catalyzer, continues vacuum hydro-extraction, and wherein, the weight ratio of catalyzer and caprolactam monomer is 0.1-2: 100;
Second step, remove vacuum, be 0-25 according to the weight ratio of polysulfone resin and caprolactam monomer: 100 ratio adding polysulfone resin, be warming up to 150 ℃-170 ℃, magnetic agitation is fully dissolved until homodisperse polysulfone resin in the hexanolactam melt, vacuum hydro-extraction once more, vacuum tightness are 10 -1-10 -3Pa;
The 3rd step, weight ratio according to activator and MC nylon monomer hexanolactam is 0-1.0: 100 ratio adds activator, be cast to after mixing rapidly in the mould that is preheated to 150-180 ℃, insulation 30min-1h postcooling promptly gets polysulfones of the present invention/MC nylon 6 composite material.
Above-mentioned polysulfone resin is polysulfones (PSU), polyethersulfone (PES), phthalein lateral group polyarylether sulfone (PES-C), contain the polyether sulphone (PPES) of naphthyridine ketone structure, contain one or more the mixture in the poly (aryl ether sulfone ketone) (PPESK) of diazanaphthalene biphenyl structure.
Above-mentioned catalyzer can be a kind of in sodium Metal 99.5, potassium metal, metallic lithium, sodium hydroxide, potassium hydroxide, yellow soda ash, all kinds of organometallic compound.
Above-mentioned activator can be a kind of in various isocyanic ester, ethanoyl hexanolactam, carbonic ether, the carboxylicesters.
After adopting such scheme, the tensile strength of the matrix material by this law preparation is 80-100MPa, modulus in tension 400-600MPa, and flexural strength 90-130MPa, bending elastic modulus 3000-4000MPa, heat-resisting decomposition temperature has improved 50-80 ℃ than pure MC.
Embodiment
Following embodiment further specifies of the present invention, and the unrestricted scope of the invention.
The anion in situ preparation method of polysulfones of the present invention/MC nylon 6 composite material, realize through the following steps:
The first step places reaction vessel to be heated to 110 ℃ the hexanolactam of 100 weight parts, vacuum hydro-extraction 30min, and vacuum is 10 -1-10 -3Pa adds 0.35 weight part sodium hydroxide as catalyzer, continues vacuum hydro-extraction 30min.
Second step, open valve, remove vacuum, add 5 weight part phthalein lateral group polyarylether sulfones, be warming up to 150 ℃, magnetic agitation is fully dissolved until homodisperse phthalein lateral group polyarylether sulfone in the hexanolactam melt.Vacuum hydro-extraction 30min, vacuum tightness is 10 -1-10 -3Pa.
The 3rd step, remove vacuum, add the activator 2.4-Xylene Diisocyanate of 0.75 weight part, be cast in the mould that is preheated to 150-180 ℃ after mixing rapidly, naturally cooling behind the insulation 1h promptly gets phthalein lateral group polyarylether sulfone/MC nylon 6 composite material.
The matrix material that makes by the present embodiment method is through electron microscope observation, phthalein lateral group polyarylether sulfone disperse phase mean sizes has only 60-100nm, and be dispersed in the matrix of nylon, its performance is as follows: tensile strength: 85MPa, modulus in tension: 480Mpa, flexural strength: 110MPa, bending elastic modulus: 3600Mpa, the temperature of thermolysis 5% improves 85 ℃ than MC nylon.

Claims (4)

1, the anion in situ preparation method of polysulfones/MC nylon 6 composite material is characterized in that: realize through the following steps:
The first step is heated to 100-120 ℃ with caprolactam monomer in reaction vessel, make material melting, vacuum hydro-extraction, and vacuum tightness is 10 -1-10 -3Pa adds catalyzer, continues vacuum hydro-extraction, and wherein, the weight ratio of catalyzer and caprolactam monomer is 0.1-2: 100;
Second step, remove vacuum, be 0-25 according to the weight ratio of polysulfone resin and caprolactam monomer: 100 ratio adding polysulfone resin, be warming up to 150 ℃-170 ℃, magnetic agitation is fully dissolved until homodisperse polysulfone resin in the hexanolactam melt, vacuum hydro-extraction once more, vacuum tightness are 10 -1-10 -3Pa;
The 3rd step, weight ratio according to activator and MC nylon monomer hexanolactam is 0-1.0: 100 ratio adds activator, be cast to after mixing rapidly in the mould that is preheated to 150-180 ℃, insulation 30min-1h postcooling promptly gets polysulfones of the present invention/MC nylon 6 composite material.
2, the anion in situ preparation method of polysulfones according to claim 1/MC nylon 6 composite material is characterized in that: above-mentioned polysulfone resin is polysulfones, polyethersulfone, phthalein lateral group polyarylether sulfone, contain the polyether sulphone of naphthyridine ketone structure, contain one or more the mixture in the poly (aryl ether sulfone ketone) of diazanaphthalene biphenyl structure.
3, the anion in situ preparation method of polysulfones according to claim 1/MC nylon 6 composite material is characterized in that: above-mentioned catalyzer can be a kind of in sodium Metal 99.5, potassium metal, metallic lithium, sodium hydroxide, potassium hydroxide, yellow soda ash, all kinds of organometallic compound.
4, the anion in situ preparation method of polysulfones according to claim 1/MC nylon 6 composite material is characterized in that: above-mentioned activator can be a kind of in various isocyanic ester, ethanoyl hexanolactam, carbonic ether, the carboxylicesters.
CNB2006100401695A 2006-04-30 2006-04-30 Anion in situ preparation method of polysulfone analog/MC nylon6 composite material Expired - Fee Related CN100516141C (en)

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CNB2006100401695A CN100516141C (en) 2006-04-30 2006-04-30 Anion in situ preparation method of polysulfone analog/MC nylon6 composite material

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Application Number Priority Date Filing Date Title
CNB2006100401695A CN100516141C (en) 2006-04-30 2006-04-30 Anion in situ preparation method of polysulfone analog/MC nylon6 composite material

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CN1865351A true CN1865351A (en) 2006-11-22
CN100516141C CN100516141C (en) 2009-07-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109796758A (en) * 2019-01-31 2019-05-24 中平神马江苏新材料科技有限公司 A kind of PA66 modified material and preparation method thereof that stability is good

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109796758A (en) * 2019-01-31 2019-05-24 中平神马江苏新材料科技有限公司 A kind of PA66 modified material and preparation method thereof that stability is good

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Granted publication date: 20090722

Termination date: 20100430