CN110330641A - A kind of preparation method of nylon resin - Google Patents
A kind of preparation method of nylon resin Download PDFInfo
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- CN110330641A CN110330641A CN201910490115.6A CN201910490115A CN110330641A CN 110330641 A CN110330641 A CN 110330641A CN 201910490115 A CN201910490115 A CN 201910490115A CN 110330641 A CN110330641 A CN 110330641A
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- nylon resin
- resin according
- acid
- diacid
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- 239000004677 Nylon Substances 0.000 title claims abstract description 37
- 229920001778 nylon Polymers 0.000 title claims abstract description 37
- 239000011347 resin Substances 0.000 title claims abstract description 36
- 229920005989 resin Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 claims abstract description 16
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920000305 Nylon 6,10 Polymers 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 19
- 239000003963 antioxidant agent Substances 0.000 claims description 15
- 230000003078 antioxidant effect Effects 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 238000010348 incorporation Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 235000015511 Liquidambar orientalis Nutrition 0.000 claims description 5
- 239000004870 Styrax Substances 0.000 claims description 5
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 5
- 235000013539 calcium stearate Nutrition 0.000 claims description 5
- 239000008116 calcium stearate Substances 0.000 claims description 5
- 238000006073 displacement reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 238000005453 pelletization Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 244000028419 Styrax benzoin Species 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- WMRCTEPOPAZMMN-UHFFFAOYSA-N 2-undecylpropanedioic acid Chemical compound CCCCCCCCCCCC(C(O)=O)C(O)=O WMRCTEPOPAZMMN-UHFFFAOYSA-N 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid group Chemical group C(C1=CC=CC=C1)(=O)O WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 20
- 239000005711 Benzoic acid Substances 0.000 description 10
- 235000010233 benzoic acid Nutrition 0.000 description 10
- -1 amido silicon Chemical compound 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 241000736148 Styrax Species 0.000 description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 4
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 2
- 229920000571 Nylon 11 Polymers 0.000 description 2
- 229920000299 Nylon 12 Polymers 0.000 description 2
- 229920000572 Nylon 6/12 Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The present invention relates to a kind of preparation method of nylon resin, which is uniformly mixed by pentanediamine, decanedioic acid, dodecanedicarboxylic acid, caprolactam by different proportions, and addition additive carries out polymerization reaction and nylon resin is made；The nylon powder product as made from this product has fusing point moderate, is easy to construct, meanwhile, in addition to having the characteristics that conventional nylon powder and being generally configured with, also have crystallization rate fast, coating gloss is high, shrinking percentage is low, coating good toughness, the advantages that transparency is high.
Description
Technical field
The invention belongs to nylon material technical field, in particular to a kind of preparation method of nylon resin.
Background technique
The existing resin for preparing nylon powder is mainly modified by nylon 11, nylon 12, nylon 610 modified resin, nylon 612
Resin or nylon 1010 or the preparation of Nylon 1012 modified resin, due to foreign technology monopolization, the country lacks former for nylon 11, nylon 12
Material can only be prepared by nylon 610 modified resin, nylon 612 modified resin or nylon 1010 or Nylon 1012 modified resin, and state
The preparation of interior nylon resin generallys use hexamethylene diamine and is modified to it, to reduce the fusing point of nylon resin, meets nylon powder application
Requirement.However, in recent years, since the production technology of the raw material of hexamethylene diamine oneself two eyeballs is only grasped by external several companies,
Additionally, due to uncontrollable factor, price remains high for a long time, and product supplies frequent fluctuation, the timely confession to nylon powder resin
Certain difficulty should be brought, unfavorable situation out of stock in spite of rising price is caused.
Summary of the invention
The technical issues of solution: the application is mainly to propose a kind of preparation method of nylon resin, is solved in the prior art
Existing foreign technology monopolization, the country lack raw material and the price technical problems such as high for a long time, are easy to get with raw material, cost
Low, function admirable is convenient for the characteristics of preparing.
Technical solution:
A kind of preparation method of nylon resin, includes the following steps:
Step 1: weighing pentanediamine by mass fraction proportion: diacid: caprolactam=(24 ~ 32): (54 ~ 65): (5 ~ 20)；
Step 2: pentanediamine, diacid and caprolactam are uniformly mixed to obtain mixture, addition mixture total mass 2.1-7.5%'s
Additive；
Step 3: mixture and additive are uniformly mixed, autoclave, sealing are put into, air in kettle is arranged in nitrogen displacement
Out, inflated with nitrogen is to 0.05-0.2MPa, and heating, when material temperature rises to 200 DEG C or more, pressure starts heat-insulation pressure keeping when reaching 1.2MPa,
Time 2 h；
Step 4: then uniformly letting out pressure to normal pressure in 2 hours, and keep the temperature 2 hours under normal pressure；
Step 5: being filled with nitrogen to 0.2MPa, outlet valve is opened, material, which is infused, takes the lead, cold rinse bank, pelleter pelletizing, through vacuum
Drying is to get finished product.
As a preferred technical solution of the present invention: the diacid in the first step is in decanedioic acid and dodecanedioic acid
One or two.
As a preferred technical solution of the present invention: diacid is decanedioic acid, the pentanediamine: the last of the ten Heavenly stems two in the first step
Acid: the mass fraction proportion of caprolactam is (26 ~ 32): (54 ~ 63): (5 ~ 20).
As a preferred technical solution of the present invention: in the first step diacid be dodecanedioic acid, the pentanediamine:
Dodecanedioic acid: the mass fraction proportion of caprolactam is (24 ~ 30): (56 ~ 65): (5 ~ 20).
As a preferred technical solution of the present invention: mixing velocity is 1000-1500r/min in the second step, is mixed
The conjunction time is 3-5min, and mixing velocity is 1500-2000r/min in third step, incorporation time 2-4min, pressure release in the 4th step
Speed is 0.05-0.15MPa/10min, is dried under vacuum to moisture content < 0.5% in the 5th step.
As a preferred technical solution of the present invention: additive is antioxidant, brightener, at surface in the second step
Manage agent and molecular weight regulator.
As a preferred technical solution of the present invention: the antioxidant is compound antioxidant, is by mass fraction proportion
Phosphorous acid: antioxidant 1010: irgasfos 168=(1 ~ 5): (5 ~ 10): (5 ~ 10), additional amount are the 1 ~ 3% of mixture total mass.
As a preferred technical solution of the present invention: the brightener is compounding brightener, is by mass fraction proportion
Acrylate leveling agent: styrax: calcium stearate=(0.1 ~ 0.5): (1 ~ 5): (1 ~ 5), additional amount are mixture total mass
0.5~2%。
As a preferred technical solution of the present invention: the surface treating agent is amino modified or polyether-modified water-soluble
Property silicone oil, additional amount be mixture total mass 0.5 ~ 2%.
As a preferred technical solution of the present invention: the molecular weight regulator is benzoic acid, and additional amount is mixture
The 0.1 ~ 0.5% of gross mass.
The utility model has the advantages that the preparation method of herein described nylon resin is compared with the prior art by using the above technical solution,
It has following technical effect that
1, the pentanediamine prepared using biofermentation technique realizes whole production domesticization of synthetic nylon resin raw material, not only Buddhist nun
The performance of imperial resin than originally gets a promotion, and also reduces production cost, it is ensured that raw material it is in liberal supply.
2, it is easy to get with raw material, at low cost, function admirable is convenient for the characteristics of preparing.
3,170 ~ 188 DEG C of product fusing point, melt index (230 DEG C, 2.16kg): 36-45 grams/10 minutes, (shore was hard for hardness
Degree): 70-78, elongation at break: 400-500%, toughness: batten doubling is continuous, resilience: after batten doubling, unclamping, batten is multiple
It is former.
4, tensile strength 60-80MPa, bending strength 80-100MPa, notch impact strength 50-60J/m, wearability and resistance to
Acid and alkali corrosion performance is good, and wearability coefficient of friction is high lower than 0.18, PV value, and Taber Abrasion 1.5-3.5mg/1000 times passes through
DIN53754 measures abrasion loss 1.5-3.5mg, and self-lubrication is good and salt spray resistance, oil resistant, resistance to -60 DEG C of low temperature.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of preparation method of nylon resin, includes the following steps:
Step 1: weighing 78 kilograms of pentanediamine by mass fraction proportion, 162 kilograms of decanedioic acid, 60 kilograms of caprolactam, resist
4.5 kilograms of oxygen agent, 1.5 kilograms of brightener, 1 kilogram of amido silicon oil, 600 grams of benzoic acid, the antioxidant by 500 grams of phosphorous acid,
Antioxidant 1010 is 2 kilograms and irgasfos 168 is 2 kilograms and compounds that the brightener is by 500 grams of calcium stearate, acrylic acid
500 grams and 500 grams of styrax of ester levelling agent compound；
Step 2: pentanediamine, decanedioic acid and caprolactam are uniformly mixed to obtain mixture, mixing velocity 1000-1500r/
Min, incorporation time 3-5min, addition antioxidant, brightener, amido silicon oil and benzoic acid；
Step 3: mixture, antioxidant, brightener, amido silicon oil and benzoic acid are uniformly mixed, mixing velocity 1500-
2000r/min, incorporation time 2-4min, put into autoclave, sealing, and nitrogen displacement air in kettle is discharged, inflated with nitrogen
To 0.2MPa, heating, when material temperature rises to 200 DEG C or more, pressure starts heat-insulation pressure keeping, time 2 h when reaching 1.2MPa；
Step 4: then uniformly letting out pressure in 2 hours to normal pressure, pressure release speed is 0.1MPa/10min, and under normal pressure
Heat preservation 2 hours；
Step 5: being filled with nitrogen to 0.2MPa, outlet valve is opened, material, which is infused, takes the lead, cold rinse bank, pelleter pelletizing, through vacuum
It is dry, moisture content < 0.5% is dried under vacuum to get finished product.
Product index is as follows:
Fusing point: 170 ~ 180 DEG C
Melt index (230 DEG C, 2.16kg): 40 grams/10 minutes
Hardness (shore hardness): 75
Elongation at break: 400%
Toughness: batten doubling is continuous
Resilience: it after batten doubling, unclamps, batten restores.
Embodiment 2
A kind of preparation method of nylon resin, includes the following steps:
Step 1: weighing 90 kilograms of pentanediamine by mass fraction proportion, 195 kilograms of dodecanedioic acid, caprolactam 15 is public
Jin, 3.5 kilograms of antioxidant, 2 kilograms of brightener, 0.5 kilogram of amido silicon oil, 800 grams of benzoic acid, the antioxidant is by phosphorous acid
500 grams, antioxidant 1010 is 2 kilograms and irgasfos 168 is 1 kilogram and compounds that the brightener is by calcium stearate 500
Gram, 1000 grams of acrylate leveling agent and 500 grams of styrax compound；
Step 2: pentanediamine, dodecanedioic acid and caprolactam are uniformly mixed to obtain mixture, mixing velocity 1000-
1500r/min, incorporation time 3-5min, addition antioxidant, brightener, amido silicon oil and benzoic acid；
Step 3: mixture, antioxidant, brightener, amido silicon oil and benzoic acid are uniformly mixed, mixing velocity 1500-
2000r/min, incorporation time 2-4min, put into autoclave, sealing, and nitrogen displacement air in kettle is discharged, inflated with nitrogen
To 0.2MPa, heating, when material temperature rises to 200 DEG C or more, pressure starts heat-insulation pressure keeping, time 2 h when reaching 1.2MPa；
Step 4: then uniformly letting out pressure in 2 hours to normal pressure, pressure release speed is 0.1MPa/10min, and under normal pressure
Heat preservation 2 hours；
Step 5: being filled with nitrogen to 0.2MPa, outlet valve is opened, material, which is infused, takes the lead, cold rinse bank, pelleter pelletizing, through vacuum
Dry, drying is to moisture content < 0.5% to get finished product.
Product index is as follows:
Fusing point: 182 ~ 188 DEG C
Melt index (230 DEG C, 2.16kg): 45 grams/10 minutes
Hardness (shore hardness): 78
Elongation at break: 440%
Toughness: batten doubling is continuous
Resilience: it after batten doubling, unclamps, batten restores.
Embodiment 3
A kind of preparation method of nylon resin, includes the following steps:
Step 1: 78 kilograms of pentanediamine are weighed by mass fraction proportion, and 140 kilograms of decanedioic acid, 22 kilograms of dodecanedioic acid,
It is 60 kilograms of caprolactam, 3 kilograms of antioxidant, 1.5 kilograms of brightener, 1.5 kilograms of amido silicon oil, 500 grams of benzoic acid, described anti-
Oxygen agent by 500 grams of phosphorous acid, 2 kilograms of antioxidant 1010 and irgasfos 168 be 0.5 kilogram compound, the brightener by
500 grams of calcium stearate, 500 grams of acrylate leveling agent and 500 grams of styrax compound；
Step 2: pentanediamine, decanedioic acid and caprolactam are uniformly mixed to obtain mixture, mixing velocity 1000-1500r/
Min, incorporation time 3-5min, addition antioxidant, brightener, amido silicon oil and benzoic acid；
Step 3: mixture, antioxidant, brightener, amido silicon oil and benzoic acid are uniformly mixed, mixing velocity 1500-
2000r/min, incorporation time 2-4min, put into autoclave, sealing, and nitrogen displacement air in kettle is discharged, inflated with nitrogen
To 0.2MPa, heating, when material temperature rises to 200 DEG C or more, pressure starts heat-insulation pressure keeping, time 2 h when reaching 1.2MPa；
Step 4: then uniformly letting out pressure in 2 hours to normal pressure, pressure release speed is 0.1MPa/10min, and under normal pressure
Heat preservation 2 hours；
Step 5: being filled with nitrogen to 0.2MPa, outlet valve is opened, material, which is infused, takes the lead, cold rinse bank, pelleter pelletizing, cold rinse bank
For cooling down material, brittle state is cooled to by soft tough state, is convenient for blank, it is big to control resin particle for pelleter revolving speed speed
It is small, it is vacuum dried, moisture content < 0.5% is dried under vacuum to get finished product.
Product index is as follows:
Fusing point: 175 ~ 185 DEG C
Melt index (230 DEG C, 2.16kg): 36 grams/10 minutes
Hardness (shore hardness): 70
Elongation at break: 500%
Toughness: batten doubling is continuous
Resilience: it after batten doubling, unclamps, batten restores.
According to above-mentioned Testing index, the novel nylon resin of synthesis fully meets and prepares nylon powder nylon resin
Requirement, and be easy to get with raw material, advantage low in cost.
Claims (10)
1. a kind of preparation method of nylon resin, it is characterised in that include the following steps:
Step 1: weighing pentanediamine by mass fraction proportion: diacid: caprolactam=(24 ~ 32): (54 ~ 65): (5 ~ 20)；
Step 2: pentanediamine, diacid and caprolactam are uniformly mixed to obtain mixture, addition mixture total mass 2.1-7.5%'s
Additive；
Step 3: mixture and additive are uniformly mixed, autoclave, sealing are put into, air in kettle is arranged in nitrogen displacement
Out, inflated with nitrogen is to 0.05-0.2MPa, and heating, when material temperature rises to 200 DEG C or more, pressure starts heat-insulation pressure keeping when reaching 1.2MPa,
Time 2 h；
Step 4: then uniformly letting out pressure to normal pressure in 2 hours, and keep the temperature 2 hours under normal pressure；
Step 5: being filled with nitrogen to 0.2MPa, outlet valve is opened, material, which is infused, takes the lead, cold rinse bank, pelleter pelletizing, through vacuum
Drying is to get finished product.
2. the preparation method of nylon resin according to claim 1, it is characterised in that: the diacid in the first step is the last of the ten Heavenly stems two
One or both of acid and dodecanedioic acid.
3. the preparation method of nylon resin according to claim 2, it is characterised in that: diacid is the last of the ten Heavenly stems two in the first step
Acid, the pentanediamine: decanedioic acid: the mass fraction proportion of caprolactam is (26 ~ 32): (54 ~ 63): (5 ~ 20).
4. the preparation method of nylon resin according to claim 2, it is characterised in that: diacid is 12 carbon in the first step
Diacid, the pentanediamine: dodecanedioic acid: the mass fraction proportion of caprolactam is (24 ~ 30): (56 ~ 65): (5 ~ 20).
5. the preparation method of nylon resin according to claim 2, it is characterised in that: mixing velocity is in the second step
1000-1500r/min, incorporation time 3-5min, mixing velocity is 1500-2000r/min, incorporation time 2- in third step
4min, pressure release speed is 0.05-0.15MPa/10min in the 4th step, is dried under vacuum to moisture content < 0.5% in the 5th step.
6. the preparation method of nylon resin according to claim 2, it is characterised in that: additive is antioxygen in the second step
Agent, brightener, surface treating agent and molecular weight regulator.
7. the preparation method of nylon resin according to claim 6, it is characterised in that: the antioxidant is compound antioxidant,
Be phosphorous acid by mass fraction proportion: antioxidant 1010: irgasfos 168=(1 ~ 5): (5 ~ 10): (5 ~ 10), additional amount are mixed
Close the 1 ~ 3% of material gross mass.
8. the preparation method of nylon resin according to claim 6, it is characterised in that: the brightener is compounding brightener,
It is acrylate leveling agent: styrax: calcium stearate=(0.1 ~ 0.5): (1 ~ 5): (1 ~ 5), additional amount by mass fraction proportion
It is the 0.5 ~ 2% of mixture total mass.
9. the preparation method of nylon resin according to claim 6, it is characterised in that: the surface treating agent changes for amino
Property or polyether-modified water-soluble silicon oil, additional amount be mixture total mass 0.5 ~ 2%.
10. the preparation method of nylon resin according to claim 6, it is characterised in that: the molecular weight regulator is benzene first
Acid, additional amount are the 0.1 ~ 0.5% of mixture total mass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910490115.6A CN110330641B (en) | 2019-06-06 | 2019-06-06 | Preparation method of nylon resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910490115.6A CN110330641B (en) | 2019-06-06 | 2019-06-06 | Preparation method of nylon resin |
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| CN110330641A true CN110330641A (en) | 2019-10-15 |
| CN110330641B CN110330641B (en) | 2021-07-06 |
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| CN201910490115.6A Active CN110330641B (en) | 2019-06-06 | 2019-06-06 | Preparation method of nylon resin |
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| US20140336353A1 (en) * | 2013-03-15 | 2014-11-13 | E I Du Pont De Nemours And Company | New polymers derived from renewably resourced lysinol |
| CN104962229A (en) * | 2015-06-25 | 2015-10-07 | 上海天洋热熔粘接材料股份有限公司 | Preparing method for polyamide hot melt adhesive |
| CN105238336A (en) * | 2015-11-13 | 2016-01-13 | 上海天洋热熔粘接材料股份有限公司 | Special copolyamide hot melt adhesive for low-surface energy coated aluminum-plastic panel and preparation method of special copolyamide hot melt adhesive |
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2019
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| CN102863616A (en) * | 2012-06-16 | 2013-01-09 | 上海天洋热熔胶有限公司 | Preparation method of low-melting-point copolyamide hot melt adhesive |
| US20140336353A1 (en) * | 2013-03-15 | 2014-11-13 | E I Du Pont De Nemours And Company | New polymers derived from renewably resourced lysinol |
| CN103254868A (en) * | 2013-05-17 | 2013-08-21 | 上海凯赛生物技术研发中心有限公司 | Hot melt adhesive |
| CN104962229A (en) * | 2015-06-25 | 2015-10-07 | 上海天洋热熔粘接材料股份有限公司 | Preparing method for polyamide hot melt adhesive |
| CN105238336A (en) * | 2015-11-13 | 2016-01-13 | 上海天洋热熔粘接材料股份有限公司 | Special copolyamide hot melt adhesive for low-surface energy coated aluminum-plastic panel and preparation method of special copolyamide hot melt adhesive |
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Effective date of registration: 20240201 Address after: 211167 room 319, comprehensive service building, Nanjing Institute of technology, No.1 Hongjing Avenue, Jiangning District, Nanjing City, Jiangsu Province (Jiangning high tech Park) Patentee after: Nanjing leitaike Material Technology Co.,Ltd. Country or region after: China Address before: 1 No. 211167 Jiangsu city of Nanjing province Jiangning Science Park Hongjing Road Patentee before: NANJING INSTITUTE OF TECHNOLOGY Country or region before: China |