CN105013205A - Apparatus for preparing polyamide, pressure reducing method as well as production equipment and production method for polyamide - Google Patents
Apparatus for preparing polyamide, pressure reducing method as well as production equipment and production method for polyamide Download PDFInfo
- Publication number
- CN105013205A CN105013205A CN201510239239.9A CN201510239239A CN105013205A CN 105013205 A CN105013205 A CN 105013205A CN 201510239239 A CN201510239239 A CN 201510239239A CN 105013205 A CN105013205 A CN 105013205A
- Authority
- CN
- China
- Prior art keywords
- polyamide
- kettle
- coil pipe
- present
- production
- 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.)
- Granted
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 64
- 239000004952 Polyamide Substances 0.000 title claims abstract description 59
- 229920002647 polyamide Polymers 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 108
- 229920006141 Polyamide 5X Polymers 0.000 claims abstract description 39
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 62
- 238000006116 polymerization reaction Methods 0.000 claims description 40
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 238000006068 polycondensation reaction Methods 0.000 claims description 30
- 150000003839 salts Chemical class 0.000 claims description 21
- 229920000642 polymer Polymers 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 230000006837 decompression Effects 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 11
- 238000001704 evaporation Methods 0.000 claims description 9
- 238000012643 polycondensation polymerization Methods 0.000 claims description 9
- 230000000977 initiatory effect Effects 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 6
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- -1 copper halide Chemical class 0.000 description 19
- 239000002253 acid Substances 0.000 description 17
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 14
- 239000000654 additive Substances 0.000 description 11
- 125000001931 aliphatic group Chemical group 0.000 description 11
- 239000012071 phase Substances 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000007791 liquid phase Substances 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 7
- 239000003638 chemical reducing agent Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 238000010276 construction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 150000004985 diamines Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000007701 flash-distillation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 4
- 238000009938 salting Methods 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 239000004472 Lysine Substances 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 150000003951 lactams Chemical class 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 108090000489 Carboxy-Lyases Proteins 0.000 description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 2
- 108010048581 Lysine decarboxylase Proteins 0.000 description 2
- IPRJXAGUEGOFGG-UHFFFAOYSA-N N-butylbenzenesulfonamide Chemical compound CCCCNS(=O)(=O)C1=CC=CC=C1 IPRJXAGUEGOFGG-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 229920000305 Nylon 6,10 Polymers 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 2
- WHBMMWSBFZVSSR-UHFFFAOYSA-N R3HBA Natural products CC(O)CC(O)=O WHBMMWSBFZVSSR-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 235000001014 amino acid Nutrition 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 150000004984 aromatic diamines Chemical class 0.000 description 2
- 238000011953 bioanalysis Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000003484 crystal nucleating agent Substances 0.000 description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- 238000011143 downstream manufacturing Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000003623 enhancer Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 235000018977 lysine Nutrition 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- LQERIDTXQFOHKA-UHFFFAOYSA-N nonadecane Chemical compound CCCCCCCCCCCCCCCCCCC LQERIDTXQFOHKA-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 2
- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
- VXHBSUHNLIQCEW-JEDNCBNOSA-N (2S)-2,6-diaminohexanoic acid pentane-1,1-diamine Chemical compound CCCCC(N)N.NCCCC[C@H](N)C(O)=O VXHBSUHNLIQCEW-JEDNCBNOSA-N 0.000 description 1
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 1
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 description 1
- DGZQEAKNZXNTNL-UHFFFAOYSA-N 1-bromo-4-butan-2-ylbenzene Chemical class CCC(C)C1=CC=C(Br)C=C1 DGZQEAKNZXNTNL-UHFFFAOYSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical compound NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 description 1
- VJHDPVWEDUCKRQ-UHFFFAOYSA-N 12-aminododecanoic acid Chemical compound NCCCCCCCCCCCC(O)=O.NCCCCCCCCCCCC(O)=O VJHDPVWEDUCKRQ-UHFFFAOYSA-N 0.000 description 1
- ZUHPIMDQNAGSOV-UHFFFAOYSA-N 2-benzyl-2-phenylpropanedioic acid Chemical class C=1C=CC=CC=1C(C(=O)O)(C(O)=O)CC1=CC=CC=C1 ZUHPIMDQNAGSOV-UHFFFAOYSA-N 0.000 description 1
- PMOWTIHVNWZYFI-UHFFFAOYSA-N 2-coumaric acid Chemical compound OC(=O)C=CC1=CC=CC=C1O PMOWTIHVNWZYFI-UHFFFAOYSA-N 0.000 description 1
- MSCMTURKIQRYPE-UHFFFAOYSA-N 2-hydroxyanthracene-1-carboxylic acid Chemical compound C1=CC=C2C=C3C(C(=O)O)=C(O)C=CC3=CC2=C1 MSCMTURKIQRYPE-UHFFFAOYSA-N 0.000 description 1
- UPHOPMSGKZNELG-UHFFFAOYSA-N 2-hydroxynaphthalene-1-carboxylic acid Chemical compound C1=CC=C2C(C(=O)O)=C(O)C=CC2=C1 UPHOPMSGKZNELG-UHFFFAOYSA-N 0.000 description 1
- IOOMARWCHDJQRL-UHFFFAOYSA-N 2-hydroxyphenanthrene-1-carboxylic acid Chemical compound C1=CC2=CC=CC=C2C2=C1C(C(=O)O)=C(O)C=C2 IOOMARWCHDJQRL-UHFFFAOYSA-N 0.000 description 1
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- WHBMMWSBFZVSSR-UHFFFAOYSA-M 3-hydroxybutyrate Chemical compound CC(O)CC([O-])=O WHBMMWSBFZVSSR-UHFFFAOYSA-M 0.000 description 1
- ALRHLSYJTWAHJZ-UHFFFAOYSA-M 3-hydroxypropionate Chemical compound OCCC([O-])=O ALRHLSYJTWAHJZ-UHFFFAOYSA-M 0.000 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- KLSLBUSXWBJMEC-UHFFFAOYSA-N 4-Propylphenol Chemical compound CCCC1=CC=C(O)C=C1 KLSLBUSXWBJMEC-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
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- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241000588731 Hafnia Species 0.000 description 1
- 241000588729 Hafnia alvei Species 0.000 description 1
- 101100257194 Homo sapiens SMIM8 gene Proteins 0.000 description 1
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- 235000019766 L-Lysine Nutrition 0.000 description 1
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- FQORROGUIFBEFC-UHFFFAOYSA-N OC(=O)C1=CC([Na])=CC(C(O)=O)=C1S(O)(=O)=O Chemical compound OC(=O)C1=CC([Na])=CC(C(O)=O)=C1S(O)(=O)=O FQORROGUIFBEFC-UHFFFAOYSA-N 0.000 description 1
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- 102100024789 Small integral membrane protein 8 Human genes 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
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- QCTBMLYLENLHLA-UHFFFAOYSA-N aminomethylbenzoic acid Chemical compound NCC1=CC=C(C(O)=O)C=C1 QCTBMLYLENLHLA-UHFFFAOYSA-N 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
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- 125000000129 anionic group Chemical group 0.000 description 1
- FNGGVJIEWDRLFV-UHFFFAOYSA-N anthracene-1,2-dicarboxylic acid Chemical class C1=CC=CC2=CC3=C(C(O)=O)C(C(=O)O)=CC=C3C=C21 FNGGVJIEWDRLFV-UHFFFAOYSA-N 0.000 description 1
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- 239000002216 antistatic agent Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- PGEAEAYLSCKCCO-UHFFFAOYSA-N benzene;n-methylmethanamine Chemical compound CNC.C1=CC=CC=C1 PGEAEAYLSCKCCO-UHFFFAOYSA-N 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
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- 230000000975 bioactive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VCCBEIPGXKNHFW-UHFFFAOYSA-N biphenyl-4,4'-diol Chemical group C1=CC(O)=CC=C1C1=CC=C(O)C=C1 VCCBEIPGXKNHFW-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910000435 bromine oxide Inorganic materials 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
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- 238000006482 condensation reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 description 1
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
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- 229940070710 valerate Drugs 0.000 description 1
Landscapes
- Polyamides (AREA)
Abstract
The present invention provides a pressure reducing apparatus for preparing polyamide.The pressure reducing apparatus comprises a sealed kettle body. The kettle body is provided with a material inlet and a material outlet, wherein the material inlet is formed above the material outlet; inside the reactor body is provided with a material coil connected with the material inlet and the material outlet; the material coil is divided into a plurality of sections; the diameters of the same sections of the material coil are the same; the diameters of different sections of the material coil are gradually increased from the material inlet to the material outlet. The present invention further provides a pressure reducing method as well as production equipment and a production method for polyamide 5X. The pressure reducing apparatus provided by the present invention is capable of effectively separating water from a material, and is good in separation effect. The production equipment and the production method for polyamide 5X provided by the present invention are specific to polyamide 5X, are capable of producing many types of polyamide 5X products, and can broaden the production and application ranges of the polyamide 5X products.
Description
Technical field
The present invention relates to field of polyamides, be specifically related to a kind of device for the preparation of polyamide, decompression method, comprise the polyamide production equipment of described device, and a kind of production method of polyamide.
Background technology
In prior art, the polymerization of polyamide generally can be divided into and add thermal polycondensation or interface polycondensation.Such as: (Bacon Ke, A.W.Sisko, Differential thermal analysis of high polymers.III.Polyamides, Journal of Polymer Science the 50th volume the 153rd phase, 87th – 98 pages, in March, 1961) describe and add thermal polycondensation process, but, according to report, add thermal polycondensation process compared to interface polycondensation, obtained polyamide fusing point low and heat resistance deterioration (J.Polym.Sci.50,87,1961; Macromolecules, 30,8540,1998).And interface polycondensation operation is very complicated, be difficult to industrially be suitable for.Above-mentioned technique is all short distance polymerization technique, no matter all there is certain defect in which kind of technique, and obtained polyamide, particularly the polyamide 5X degree of polymerization is not high, and commercial Application is very restricted.
Along with the development of polymerization technique, continuous polymerization technique arises at the historic moment, and compensate for the defect of short distance polymerization to a certain extent.Continuous polymerization technique main in the world specifically mainly comprises following link at present: concentrated → high pressure pre-polymerization → flash distillation → normal pressure or vacuum polycondensation.E.I.Du Pont Company, as polyamide manufacturer well-known in world wide, improves the continuous polymerization technique of polyamide 66, and the continuous polymerization technique of its uniqueness mainly comprises following link: high pressure concentrates pre-polymerization → flash distillation → normal pressure polycondensation.
In continuous polymerization technique, by the acting in conjunction of each group of equipment, heat is applied to reactant mixture and water is little by little removed, to drive molecular balance towards polyamide, until polymer reaches required length range, be extruded into pellet more afterwards, be spun into fiber or be processed as other shape.Whole continuous polymerization technique needs a large amount of heats, occurs to make condensation reaction and removes water from reactant mixture.
In above-mentioned polymerization technique, the flash steps of solution can use flash vessel.Flash vessel conventional in industry is vertical flash vessel, and comprising: kettle, the top of kettle is provided with steam (vapor) outlet, and the bottom of kettle is provided with feed tube, and the lower sides of kettle arranges taphole.The operation principle of vertical flash vessel is: pyrosol enters in kettle through feed tube, after pyrosol enters kettle, a temperature difference and pressure differential is produced with the air in kettle, thus pyrosol is seethed with excitement immediately and produces a large amount of steam, the steam flashed off rises, and finally discharges from steam (vapor) outlet and is separately used as him.Above-mentioned flash vessel is when flash distillation, and solution concentration constantly increases, and causes viscosity constantly to increase, easily blocks flash vessel, and flash evaporation effect is not very desirable.
Summary of the invention
For overcoming the defect that in existing polyamide production technology, decompressor exists, an object of the present invention is to provide a kind of device for the preparation of polyamide.
Second object of the present invention is to provide a kind of decompression method for the preparation of polyamide.
3rd object of the present invention is to provide the production equipment of a kind of polyamide 5X.
4th object of the present invention is to provide the production method of a kind of polyamide 5X.
Device for the preparation of polyamide provided by the invention is decompressor, comprise the kettle of sealing, described kettle is provided with material inlet, material outlet, described material inlet is positioned at the top of described material outlet, the material coil pipe be connected between described material inlet and material outlet is provided with in described kettle, described material coil pipe is divided into some sections, the described material coil diameter of same section is identical, and the described material coil pipe of different section is increased to described material outlet place diameter gradually by described material inlet.
In device of the present invention, the diameter of described material coil pipe is 20 ~ 80mm, draw ratio 600 ~ 26000.
In device of the present invention, the total length of described material coil pipe is 50 ~ 500m.
In device of the present invention, described material coil pipe is in horizontal Multi-layers distributing in described kettle, and every layer of material coil pipe is that serpentine back and forth arranges.
In device of the present invention, in described kettle, being also provided with one or more groups tube sheet, often organizing on tube sheet and be provided with perforate, passing wherein with fixing described material coil pipe for making described material coil pipe.
In device of the present invention, described kettle also comprises heating agent entrance and heating agent outlet, and described heating agent entrance is arranged at described kettle top, and described heating agent outlet is arranged at described autoclave body bottom.
In device of the present invention, described kettle also comprises one or more exhaust outlet.
Decompression method for the preparation of polyamide provided by the invention for: adopt the device described in above any one of technical scheme to carry out decompression process.
The production equipment of polyamide 5X provided by the invention comprises: the raw material enrichment facility connected successively, pre-polymerization device, decompressor, Moisture separation device and polycondensation device, and wherein, described decompressor is the device described in above any one of technical scheme.
The production method of polyamide 5X provided by the invention is: adopt aforesaid production equipment, with the polyamide salt aqueous solution for initiation material, obtain described polyamide 5X through raw material concentration step, prepolymerization step, depressurization steps, moisture separating step and condensation polymerization step successively.
In production method of the present invention, the mass percent concentration of described polyamide salt aqueous solution initiation material is more than 50%, is preferably 50 ~ 65%.
In production method of the present invention, described raw material concentration step adopts pipe shell type heat exchange device to carry out evaporation and concentration, and tube side pressure is 0.005 ~ 0.35MPa, preferably 0.05 ~ 0.35MPa, and tube side temperature is 60 ~ 200 DEG C, is preferably 80 ~ 160 DEG C; And/or
Shell side pressure is 0 ~ 2.0MPa, and uneven shell-side temperature is less than 250 DEG C, is preferably less than 212 DEG C; And/or
The mass percent concentration of the polyamide salt aqueous solution after concentrated is 50 ~ 80%, is preferably 70 ~ 80%.
In production method of the present invention, the temperature of described prepolymerization step is 200 ~ 300 DEG C, is preferably 220 ~ 280 DEG C, is more preferably 230 ~ 260 DEG C; And/or
The pressure of described prepolymerization step is below 3.0MPa, is preferably below 2.0MPa, is more preferably 1.0 ~ 1.8Mpa; And/or
The mass percentage content that described prepolymerization step terminates the polymer of rear gained is 80 ~ 100%, is preferably 85 ~ 95%.
In production method of the present invention, in described depressurization steps, in described depressurization steps, temperature is the temperature of more than described polyamide 5X fusing point, is preferably 200 ~ 300 DEG C, is more preferably 230 ~ 260 DEG C.
In production method of the present invention, in described moisture separating step, temperature is 250 ~ 320 DEG C, is preferably 250 ~ 300 DEG C.
In production method of the present invention, the temperature of described condensation polymerization step is 250 ~ 320 DEG C, is preferably 250 ~ 300 DEG C; And/or
Described condensation polymerization step is carried out under normal pressure or vacuum condition, adopts inert gas shielding when carrying out polycondensation under normal pressure, and when carrying out polycondensation under vacuum condition, pressure is 0 ~ 760mmHgA, is preferably 150 ~ 250mmHgA.
In production method of the present invention, described polyamide 5X is polyamide 56.
Decompressor provided by the invention can realize material by the setting of material coil diameter and reduce pressure wherein, thus the moisture in material can be made to become gas phase fast, be separated with liquid material, good separating effect, the moisture separating effect that downstream processing unit reaches good can be ensured, decompressor structure of the present invention is simple, and security is good, effectively can reduce production cost.
Decompression method effect of easing stress provided by the invention is good, moisture and feed separation abundant, thus ensure that integrality and the high efficiency of bulk polymerization technique.
Polyamide 5X production equipment provided by the invention have employed decompressor provided by the invention, ensure that decompression production link wherein, is especially applicable to the production of polyamide 5X.
Polyamide 5X production method provided by the invention provides the production technology for polyamide 5X, can produce the polyamide 5X product of polytypic, can expand production and the range of application of polyamide 5X product, very have industrial value.
Accompanying drawing explanation
Fig. 1 is the Facad structure schematic diagram of decompressor of the present invention;
Fig. 2 is the structural representation of polyamide 5X production equipment of the present invention;
Wherein, description of reference numerals is as follows: 0, salify device; 1, raw material enrichment facility; 2, pre-polymerization device; 3, decompressor; 4, Moisture separation device; 5, polycondensation device; 31, kettle, 311, end socket; 32, material inlet; 33, material outlet; 34, material coil pipe; 35, tube sheet; 36, heating agent entrance; 37, heating agent outlet; 38, exhaust outlet.
Detailed description of the invention
One aspect of the present invention provides a kind of decompressor for the preparation of polyamide, as shown in Figure 1, decompressor of the present invention comprises the kettle 31 of a sealing, kettle 31 is provided with material inlet 32 and material outlet 33, material inlet 32 is positioned at the top of material outlet 33, in addition, the material coil pipe 34 be connected between material inlet 32 and material outlet 33 is provided with in kettle 31, material coil pipe 34 is divided into some sections, material coil pipe 34 diameter of same section is identical, and the material coil pipe 34 of different section is increased to material outlet 33 place diameter gradually by material inlet 32.
During above-mentioned decompressor work, the material pressurization after the pre-polymerization of upstream (is generally 20 ~ 25kg/cm
2) after enter in kettle 31 by material inlet 32, material flows in material coil pipe 34, be rapidly heated to higher temperature, because the diameter of material coil pipe 34 increases gradually, add the drag effect of material and coil pipe pipe friction, pressure reduces gradually, until at material outlet 33 place close to normal pressure, due to pressure drop, the at high temperature undergoes rapid expansion gasification of moisture in material, material becomes the state of gas phase and liquid phase coexist, liquid phase material is in the inwall film flow at high speed in the form of a ring of coil pipe, gaseous phase materials then flows through in the central authorities of coil pipe, pressure changes kinetic energy into simultaneously, gas, the material of liquid mixing is discharged by material outlet 33 and is entered downstream processing unit.
In an embodiment of decompressor according to the present invention, decompressor of the present invention is applicable to common polyamide 6 X series, as nylon66 fiber etc., is also applicable to polyamide 5X series, as polyamide 56 etc.In one preferred embodiment, decompressor of the present invention is especially applicable to polyamide 5X production field.
In an embodiment of decompressor according to the present invention, kettle 31 two ends are sealed by end socket 311, carry out detachable connection by flange.
In an embodiment of decompressor according to the present invention, can be 20 ~ 80mm between the diameter region of material coil pipe 34, draw ratio can be 600 ~ 26000.In one preferred embodiment, material coil pipe 34 length can be divided into three sections of equal length, is followed successively by 35mm, 45mm and 70mm by material inlet 32 is initial.
In an embodiment of decompressor according to the present invention, the total length of material coil pipe 34 can be 50 ~ 500m.
In an embodiment of decompressor according to the present invention, material coil pipe 34 is in horizontal Multi-layers distributing in kettle 31, and every layer of material coil pipe is that serpentine back and forth arranges.
In an embodiment of decompressor according to the present invention, in kettle 31, being also provided with one or more groups tube sheet 35, passing with fixture charging tray pipe 34 wherein for making material coil pipe 34.
In an embodiment of decompressor according to the present invention, kettle 31 also comprises heating agent entrance 37 and heating agent outlet 38, and heating agent entrance 37 is arranged at the top of kettle 31, and heating agent outlet 38 is arranged at the bottom of kettle 31.In one preferred embodiment, the heating agent for decompressor of the present invention is generally gas-phase heat conducting oil.Material needs amount of heat when gasifying in material coil pipe 34, the mode of preferred employing gas-phase heat conducting oil heating, passes to condensation after material coil pipe 34 through overheated heat-shift after conduction oil steam contactant charging tray pipe 34 and becomes liquid from heating agent outlet 38 outflow at the bottom of still.
In an embodiment of decompressor according to the present invention, kettle 31 also comprises one or more exhaust outlet 39, suitably can reduce the gaseous pressure in material coil pipe 34, ensures decompressor safe operation.
Second aspect of the present invention provides a kind of decompression method for the preparation of polyamide, and it adopts the decompressor described in above any one of technical scheme to carry out decompression process.
3rd aspect of the present invention provides the production equipment of a kind of polyamide 5X, as shown in Figure 2, comprise the raw material enrichment facility 1, pre-polymerization device 2, decompressor 3, Moisture separation device 4 and the polycondensation device 5 that connect successively, wherein, decompressor 3 is the decompressor described in above any one of technical scheme.
In an embodiment of production equipment according to the present invention, the upstream of raw material enrichment facility 1 can also be connected with salify device 0, for the formation of base polyamide salt, as shown in Figure 2.
The raw material enrichment facility that the present invention relates to, pre-polymerization device, Moisture separation device and polycondensation device can adopt any type of existing polyamide production field, and the present invention is not particularly limited, all can with decompressor of the present invention with the use of.
The raw material enrichment facility that can be used for production equipment of the present invention can be a concentration kettle, raw material is heating evaporation wherein, to reach desired concn, its heating source can adopt conventional external steam source, also the overheated process steam thermal source that in pre-polymerization device, tubular reactor is discharged can be adopted, vapor (steam) temperature is generally 220 ~ 280 DEG C, and concentration kettle generally adopts the concentration kettle type of shell-and-tube.Raw material enrichment facility can further include a preheating device, the material solution before concentrated can be heated in advance, and then carries out evaporation and concentration.Raw material enrichment facility can also further comprise a condensing tower, process steam recoverable heat energy after condensation that concentration kettle produces, and the raw material carried secretly in steam such as diamines etc. also can be back in concentration kettle after condensation, to reduce the loss of raw material.
The pre-polymerization device that can be used for production equipment of the present invention can be a tubular reactor, and body is serpentine arrangement, and comprise some straight sections and the bent portion of connection, monomer material is carried and heated in body, and polycondensation forms prepolymer thus.Pre-polymerization device can further include one or more, the preferred heating jacket of more than three, is used for heated Tube reactor.Pre-polymerization device further can also comprise one or more heating agent evaporimeter, is used for providing heating agent to heating jacket.The heating agent that pre-polymerization device uses can be the organic heating agent of liquid phase, the overheated liquid phase of organic heating agent is adopted to carry the gas phase heating medium for heating mode of evaporating on the spot, use gas phase heating medium for heating tubular reactor, the heating agent lime set after using is sent heating agent evaporimeter circulating-heating back to and is utilized after reclaiming.
The Moisture separation device that can be used for production equipment of the present invention can be any type of this area, comprises the separator of normal pressure or pressurization.Such as, the prepolymer being entrained with a large amount of steam directly can enter in the separator of normal pressure from decompressor, is separated by steam in this device with prepolymer, the temperature of separating step preferably 250 ~ 320 DEG C, more preferably 250 ~ 300 DEG C.The kettle of separator 4 can adopt the overheated liquid phase of organic heating agent to carry the gas phase heating medium for heating mode of evaporating on the spot.The overheated liquid phase heating agent heating out from hot Media Oven is transported under pressure the on-the-spot flash vessel of heating and carries out vacuum flashing, the gas phase heating medium for heating separator flashed off, heating agent lime set after using sends heating medium for heating stove circulating-heating back to heat medium circulation pump after being received by matchmaker's condensate liquid recycling can by liquid trap.The squeeze cylinder of separator adopts liquid phase heating medium for heating.
The polycondensation device that can be used for production equipment of the present invention can be any type of this area, comprises the separator of normal pressure or pressurization.Such as, the liquid material (being mainly prepolymer) after Moisture separation device process enters polycondensation device under the effect of polycondensation unit feeding pump, and prepolymer generates the larger whole polymers of molecular weight through being polymerized further in the polycondensation vessel of polycondensation device.The polymer generated in polycondensation device can be transported to end of extruded band via Melt Pump and carry out extruding pelletization, or delivers to screw extruder and carry out modification granulation, or delivers to and directly spin.The kettle of polycondensation device can adopt the overheated liquid phase of organic heating agent to carry the gas phase heating medium for heating mode of evaporating on the spot.The overheated liquid phase heating agent heating out from hot Media Oven is transported under pressure the on-the-spot flash vessel of heating and carries out flash distillation, the kettle of the gas phase heating medium for heating polycondensation device flashed off, heating agent lime set after using sends heating medium for heating stove circulating-heating back to heat medium circulation pump after being accepted by matchmaker's condensate liquid recycling can by liquid trap.The squeeze cylinder of polycondensation device can adopt liquid phase heating medium for heating.
4th aspect of the present invention provides the production method of a kind of polyamide 5X, adopt production equipment provided by the invention, with the polyamide salt aqueous solution for initiation material, obtain described polyamide 5X through raw material concentration step, prepolymerization step, depressurization steps, moisture separating step and condensation polymerization step successively.
In the embodiment of in accordance with the present production process, the mass percent concentration of the initiation material polyamide salt aqueous solution can be more than 50%, can be preferably 50 ~ 65%.
In the embodiment of in accordance with the present production process, in raw material concentration step, common pipe shell type heat exchange device can be adopted to carry out evaporation and concentration, wherein, tube side pressure can be 0.005 ~ 0.35MPa, be preferably 0.05 ~ 0.35MPa, tube side temperature can be 60 ~ 200 DEG C, is preferably 80 ~ 160 DEG C; Shell side pressure can be 0 ~ 2.0MPa, and uneven shell-side temperature can be less than 250 DEG C, is preferably less than 212 DEG C; After concentrated, the mass percent concentration of the polyamide salt aqueous solution of gained can be 50 ~ 80%, is preferably 70 ~ 80%.
In the embodiment of in accordance with the present production process, in prepolymerization step, the temperature of pre-polymerization can be 200 ~ 300 DEG C, is preferably 220 ~ 280 DEG C, is more preferably 230 ~ 260 DEG C; The pressure of pre-polymerization can be below 3.0MPa, is preferably below 2.0MPa, is more preferably 1.0 ~ 1.8Mpa.
In the embodiment of in accordance with the present production process, the polymer quality degree that prepolymerization step terminates rear gained can be 80 ~ 100%, is preferably 85 ~ 95%.
In the embodiment of in accordance with the present production process, depressurization steps can adopt flash vessel to carry out, temperature and pressure in flash vessel is any condition of applicable polyamide 5X and moisture flash separation, the temperature of decompression can be the temperature of more than the fusing point of polyamide 5X, be preferably 200 ~ 300 DEG C, be more preferably 230 ~ 260 DEG C.
In the embodiment of in accordance with the present production process, the temperature in moisture separating step can be 250 ~ 320 DEG C, preferably can be 250 ~ 300 DEG C.
In the embodiment of in accordance with the present production process; condensation polymerization step is carried out under normal pressure or vacuum condition; inert gas (as nitrogen etc.) protection is adopted when carrying out polycondensation under normal pressure; when carrying out polycondensation under vacuum condition, pressure can be 0 ~ 760mmHgA; be preferably 150 ~ 250mmHgA; the temperature of condensation polymerization step can be 250 ~ 320 DEG C, preferably can be 250 ~ 300 DEG C.
In the embodiment of in accordance with the present production process, polyamide 5X is preferably polyamide 56.
Polyamide production equipment of the present invention and production method are applicable to continuous polymerization technique and the batch polymerization processes of polyamide, are particularly useful for the continuous polymerization technique of polyamide.
Polyamide 5X of the present invention refers to the polyamide series matter that 1,5-pentanediamine and organic dibasic acid are formed by polycondensation reaction.
The formic acid relative viscosity of the polyamide 5X that the present invention obtains is preferably 45 ~ 100, and terminal amino group content is preferably 10 ~ 100mol/ton, is more preferably 20 ~ 60mol/ton, and the Amino End Group of too high amount at high temperature easily side reaction occurs again.
The polyamide 5X narrow molecular weight distribution that the present invention obtains, represents Mw/Mn with the polydispersity coefficient d of conventional molecular weight distribution; Mw representative take weight as the average weight-molecular mass of statistical weight:
Mn representative take quantity as the equal relative molecular mass of number of statistical weight:
The d value of the polyamide 5X that the present invention obtains is less than 2.5.
The polyamide 5X that equipment provided by the invention and method obtain can make the polyamide of various uses jointly with other polymer and/or additive.In general, the amount of polyamide 5X can account for more than 80% of polyamide quality.
Additive can be any one or a few the combination in antioxidant, heat-resisting stabilizing agent, weather resisting agent, pigment, gloss enhancer, dyestuff, crystal nucleating agent, delustering agent, plasticizer, antistatic additive, fire retardant, metal and slaine.
Wherein, heat-resisting stabilizing agent can be the existing any type in this area, include but not limited to the compound based on hindered phenol, the compound based on quinhydrones, the compound based on thiazole, the compound based on phosphorus (as phenyl-phosphonic acid), based on compound (as 2-mercaptobenzimidazole) and substitution product, copper halide and the iodine compound etc. of imidazoles.
Weather resisting agent can be the existing any type in this area, includes but not limited to resorcinol, salicylate, BTA, benzophenone and hindered amine etc.
Pigment can be the existing any type in this area, includes but not limited to cadmium sulfide, phthalocyanine and carbon black etc.
Gloss enhancer can be the existing any type in this area, includes but not limited to titanium oxide, calcium carbonate etc.
Dyestuff can be the existing any type in this area, includes but not limited to Ni Gehei and nigrosine etc.
Crystal nucleating agent can be the existing any type in this area, includes but not limited to talcum, silica, kaolin and clay etc.
Plasticizer can be the existing any type in this area, includes but not limited to oxybenzoic acid monooctyl ester and N-butylbenzenesulfonamide etc.
Antistatic additive can be the existing any type in this area, includes but not limited to alkyl sulphate type anionic antioxidant, quaternary ammonium salt cationic type antistatic additive, non-ionic antistatic agent (as Tween-60) and the both sexes antistatic additive etc. based on betaine.
Fire retardant can be the existing any type in this area, includes but not limited to melamine cyanurate, hydroxide (as magnesium hydroxide or aluminium hydroxide), ammonium polyphosphate, brominated Polystyrene, brominated polyphenylether, brominated polycarbonate, brominated epoxy resin, the combination etc. that is made up of any fire retardant based on bromine and antimony oxide.
Other polymer includes but not limited to following polymer: (1) other polymer can contain the construction unit derived from following component: aliphatic carboxylic acid is (as oxalic acid, malonic acid, butanedioic acid, glutaric acid, pimelic acid, suberic acid, azelaic acid etc.), alicyclic dicarboxylic acid (as cyclohexyl dicarboxylic acid etc.) or aromatic dicarboxylic acid are (as terephthalic acid (TPA), M-phthalic acid, naphthalenedicarboxylic acid, diphenyldicarboxylic acid, anthracene dicarboxylic acids, luxuriant and rich with fragrance dicarboxylic acids, diphenyl ether dicarboxylic acids, diphenoxyethanedicarboxylic acid, diphenylethane dicarboxylic acids, 1, 4-cyclohexyl dicarboxylic acid, 5-sodiosulfoisophthalic acid, 5-4-butyl-phosphonium M-phthalic acid etc.).
(2) other polymer can contain the construction unit derived from following component: except 1, aliphatic diamine outside 5-pentanediamine is (as ethylenediamine, 1, 3-diaminopropanes, 1, 4-diaminobutane, 1, 6-diamino hexane, 1, 7-diaminoheptane, 1, 8-diamino-octane, 1, 9-diamino nonane, 1, 10-diamino decane, 1, 11-diamino undecane, 1, 12-diamino dodecane, 1, 13-diaminourea tridecane, 1, the 14-diaminourea tetradecane, 1, 15-diaminourea pentadecane, 1, 16-diaminourea hexadecane, 1, 17-diaminourea heptadecane, 1, 18-diaminourea octadecane, 1, 19-diaminourea nonadecane, 1, 20-diaminourea eicosane or 2-methyl isophthalic acid, 5-pentanediamine), alicyclic diamine (as cyclohexanediamine or two-(4-Aminohexyl) methane) or aromatic diamine (as benzene dimethylamine).
(3) other polymer can contain the construction unit derived from following component: aromatic series, aliphatic or alicyclic diol compound are (as ethylene glycol, propane diols, butanediol, pentanediol, hexylene glycol, 1,4-cyclohexanedimethanol, neopentyl glycol, quinhydrones, resorcinol, dihydroxybiphenyl, naphthalene glycol, anthracene glycol, luxuriant and rich with fragrance glycol, 2, two (4-hydroxy phenyl) propane, 4 of 2-, 4 '-dihydroxydiphenyl ether or bisphenol S).
(4) other polymer can contain the construction unit derived from following component: have the aromatic compound of hydroxyl and carboxylic acid, aliphatic compound or cycloaliphatic hydroxyl group carboxylic acid compound.Wherein, cycloaliphatic hydroxyl group carboxylic acid includes but not limited to lactic acid, 3-hydroxy propionate, 3-hydroxybutyrate ester, 3-hydroxybutyrate ester-valerate, hydroxybenzoic acid, hydroxyl naphthalene-carboxylic acid, hydroxyl anthracene carboxylic acid, hydroxyl phenanthrene carboxylic acid, (hydroxy phenyl) vinyl carboxylic acid.
(5) other polymer can contain the construction unit derived from following component: amino acid (as 6-aminocaprolc acid, 11-amino undecanoic acid, 12 amino dodecanoic acid or PAMBA) or lactams (as epsilon-caprolactams or ε-lauric lactam).
(6) other polymer can be can with 1, the comonomer of 5-pentanediamine and the copolymerization of aliphatic long carbochain biatomic acid, this comonomer includes but not limited to amino acid, lactams, aromatic dicarboxylic acid, aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic diol, aliphatic diol, alicyclic diol, aromatic diamine, aliphatic diamine, alicyclic diamine, aromatic hydroxy-carboxylic, aliphatic hydroxyl carboxylic acid, cycloaliphatic hydroxyl group carboxylic acid, and above-mentioned comonomer derivative separately.Wherein, above-mentioned comonomer derivative separately comprises the product of above-mentioned any two kinds of comonomers reaction, such as, and the product of an amino of a part diamines and a carboxyl reaction salify of a part dicarboxylic acids.
Below by embodiment, the present invention is described in detail, to make the features and advantages of the present invention clearer.But it is noted that embodiment is for understanding design of the present invention, scope of the present invention is not limited only to listed embodiment herein.
As being not particularly illustrated, concentration of the present invention is mass percent concentration.
The polyamide initiation material that embodiment uses is the polyamide salt aqueous solution, and this polyamide salt is formed by 1,5-pentanediamine of bio-based and aliphatic dibasic acid.
[1,5-pentanediamine]
1,5-pentanediamine (is called for short pentanediamine, has another name called 1., 5-1,5-DAP), also claim cadaverine, it is a polyamine species, be extensively exist in organism there is bioactive nitrogenous base, for protein corrupt time lysine under the effect of decarboxylase, there is decarboxylic reaction generate.Industrial pentanediamine also can pass through chemical method, such as, after being boiled by the ethanol solution of glutaronitrile, adds sodium metal with speed faster, add water after having reacted, steamed by ethanol, remaining reactant superheated steam distills, acidizing neutralization again, the method for distillation obtains.The bioanalysis that the discovered in recent years pentanediamine lysine decarboxylase (L-lysine decarboxylase, EC 4.1.1.18) that can pass through in hafnia alvei (Hafnia.Alvei) acts on lysine obtains.1,5-pentanediamine of the embodiment of the present invention can be formed by Biological preparation, also can be prepared from by chemical method, and can containing the organic carbon of renewable source meeting ASTM D6866 standard.
[aliphatic dibasic acid]
Aliphatic dibasic acid, comprises adipic acid and aliphatic long carbochain biatomic acid.Aliphatic long carbochain biatomic acid also can be prepared from by bioanalysis or chemical method, and also can containing the bio-based organic carbon meeting ASTM D6866 standard.
Aliphatic long carbochain biatomic acid can be decanedioic acid, DC11, SL-AH, tridecanyldicarboxylic acid, DC14,15 carbon dicarboxylic acids, 16-dicarboxylic acid, DC17, DC18 and △ 9-1, any one or a few combination in 18-octadecylene binary acid, is preferably decanedioic acid or SL-AH.
The continuous flow procedure of polyamide is as follows:
(1) preparation of polyamide salt solution
Under the protection of nitrogen, the deionized water of 1,5-pentanediamine degasification of high concentration is diluted to certain density solution (30% ~ 50%).Aliphatic dibasic acid and 1, the 5-pentanediamine diluted are joined continuously in reactor, cooling water removes reaction heat during neutralization reaction in time simultaneously.The pH value of solution is constantly detected in N-process, make the mol ratio of the diamine/binary acid in reactor a little less than 1, after stable, this gained salting liquid is transferred to (multiple stage of can connecting in the reactor of connecting below, but be generally no more than 3), the mol ratio of diamine/binary acid and the mass concentration of salt is regulated, the flow of Data Control two amine aqueous solution detected with pH with the further fractional neutralization of two amine aqueous solutions.Until finally make the salting liquid that mass percent concentration is 50 ~ 65%, leave in salt holding vessel stand-by.
(2) enrichment facility and reaction thereof
Be that the 5X polyamide salt aqueous solution of 50 ~ 65% is for initiation material with mass percent concentration, through metre filter, send into measuring tank in batches, the common additives (being generally no more than 5% of polyamide salt quality) of a certain amount of different size can be added in measuring tank, make polyamide salt mixed solution, after being uniformly mixed, be admitted to the second medial launder under measuring tank.Polyamide salt mixed liquor in second medial launder is supplied in enrichment facility by salt filter, salt preheater continuous print by salt supply pump.In enrichment facility, polyamide salt solution concentration is made to be concentrated to 70 ~ 80% by 50 ~ 65%.
(3) pre-polymerization device and reaction thereof
Concentrate reactor supply pump in enrichment facility is delivered in pre-polymerization device.
Prepolymerization reaction flows through continuously with polyamide saline solution and occurs gradually under controllable HTHP in tubular reactor.During this, the pressure of reactor automatically controls, tubular reactor is divided into more than three sections independent heatings, still with simmer down to master in the tubular reactor of first 2/3 section, solution concentration is concentrated to about 90% (being suitable for carrying out the concentration of polymerisation) by 70 ~ 80%, final stage is combined into master to carry out pre-polymerization, and in the material of outlet, polymer content can reach 85 ~ 95%.
(4) decompressor and reaction thereof
Pressure reducer (flash vessel) given continuously by the prepolymer pressure reducer pump obtained by tubular reactor.Material is rapidly by pressure reducer, and pressure reduces continuously and close to atmospheric pressure, so the dissolved water in prepolymer gasifies rapidly from prepolymer, forms the mixture of material, moisture.
Pipeline between pressure reducer pump and pressure reducer can also be provided with additive and add entrance, such as, according to kind and addition, the delustering agent TiO of the purposes determination additive of PA5X resin
2suspension etc., add entrance by additive, can be injected into continuously and quantitatively in prepolymer in this stage, after being reduced pressure by decompressor, finally form the mixture of material, moisture and additive.
(5) separator and reaction thereof
Material continuous print after pressure reducer enters water-separator.The moisture removing of gasifying out from pressure reducer in separator, improve the degree of polymerization of prepolymer further.
(6) poly-device and reaction thereof eventually
With amounting to pump, the material by separator is sent in whole poly-device (terminal polymerization kettle); in whole poly-device; Residual water in polymer and the water that produces of polymerization is further removed, the high quality polymer obtaining applicable granulation or modification or directly spin under condition of negative pressure.In order to prevent separator, terminal polymerization kettle material to be oxidized, preferably adopt nitrogen-sealed.
Be below the embodiment of preparation PA56:
Embodiment 1
Configuration pH is polyamide 56 salting liquid of 65% concentration of 7.95, and be polymerized by the process conditions of production equipment of the present invention by table 1, terminal polymerization kettle pressure 210mmHg A, obtains the section that relative viscosity is 68.9, and its terminal amino group content is 40.4.
Embodiment 2
Configuration pH is polyamide 56 salting liquid of 65% concentration of 8.05, be polymerized by the process conditions of production equipment of the present invention by embodiment 1, but the pressure of terminal polymerization kettle adjusts to 180mmHgA by force, load improves 20% than embodiment 1, obtain the section that relative viscosity is 69.7, its terminal amino group content is 40.1.
Embodiment 3
Except the pressure change in terminal polymerization kettle is 216mmHg A, other condition is identical with embodiment 2, and load too, obtains the section that relative viscosity is 56.1, and its terminal amino group content is 42.6.
Table 1
The explanation of above embodiment just to technical scheme, does not form the restriction to the technology of the present invention.Those skilled in the art, according to professional knowledge, can realize the polyamide of different end group content and relative viscosity by the pulp furnish in adjustment preparation process and process conditions.
Unless limited otherwise, term used herein is the implication that those skilled in the art understand usually.
Embodiment described in the invention is only for exemplary purpose; and be not used to limit the scope of the invention, those skilled in the art can make other replacements various, changes and improvements within the scope of the invention, thus; the invention is not restricted to above-mentioned embodiment, and be only defined by the claims.
Claims (17)
1. the device for the preparation of polyamide, it is characterized in that, described device is decompressor, comprise the kettle of sealing, described kettle is provided with material inlet, material outlet, described material inlet is positioned at the top of described material outlet, the material coil pipe be connected between described material inlet and material outlet is provided with in described kettle, described material coil pipe is divided into some sections, the described material coil diameter of same section is identical, and the described material coil pipe of different section is increased to described material outlet place diameter gradually by described material inlet.
2. device according to claim 1, is characterized in that, the diameter of described material coil pipe is 20 ~ 80mm, and draw ratio is 600 ~ 26000.
3. device according to claim 1, is characterized in that, the total length of described material coil pipe is 50 ~ 500m.
4. device according to claim 1, is characterized in that, described material coil pipe is in horizontal Multi-layers distributing in described kettle, and every layer of material coil pipe is that serpentine back and forth arranges.
5. device according to claim 1, is characterized in that, is also provided with one or more groups tube sheet in described kettle, often organizes on tube sheet and is provided with perforate, passes wherein for making described material coil pipe with fixing described material coil pipe.
6. device according to claim 1, is characterized in that, described kettle also comprises heating agent entrance and heating agent outlet, and described heating agent entrance is arranged at described kettle top, and described heating agent outlet is arranged at described autoclave body bottom.
7. device according to claim 1, is characterized in that, described kettle also comprises one or more exhaust outlet.
8. for the preparation of a decompression method for polyamide, it is characterized in that, adopt the device described in any one of claim 1-7 to carry out decompression process.
9. a production equipment of polyamide 5X, is characterized in that, comprises the raw material enrichment facility, pre-polymerization device, decompressor, Moisture separation device and the polycondensation device that connect successively, and wherein, described decompressor is the device described in any one of claim 1-7.
10. the production method of a polyamide 5X, it is characterized in that, adopt production equipment according to claim 9, with the polyamide salt aqueous solution for initiation material, obtain described polyamide 5X through raw material concentration step, prepolymerization step, depressurization steps, moisture separating step and condensation polymerization step successively.
11. production methods according to claim 10, is characterized in that, the mass percent concentration of described polyamide salt aqueous solution initiation material is more than 50%, are preferably 50 ~ 65%.
12. production methods according to claim 10 or 11, is characterized in that, described raw material concentration step adopts pipe shell type heat exchange device to carry out evaporation and concentration, tube side pressure is 0.005 ~ 0.35MPa, preferably 0.05 ~ 0.35MPa, tube side temperature is 60 ~ 200 DEG C, is preferably 80 ~ 160 DEG C; And/or
Shell side pressure is 0 ~ 2.0MPa, and uneven shell-side temperature is less than 250 DEG C, is preferably less than 212 DEG C; And/or
The mass percent concentration of the polyamide salt aqueous solution after concentrated is 50 ~ 80%, is preferably 70 ~ 80%.
13. production methods according to any one of claim 10-12, it is characterized in that, the temperature of described prepolymerization step is 200 ~ 300 DEG C, is preferably 220 ~ 280 DEG C, is more preferably 230 ~ 260 DEG C; And/or
The pressure of described prepolymerization step is below 3.0MPa, is preferably below 2.0MPa, is more preferably 1.0 ~ 1.8Mpa; And/or
The mass percentage content that described prepolymerization step terminates the polymer of rear gained is 80 ~ 100%, is preferably 85 ~ 95%.
14. production methods according to any one of claim 10-13, it is characterized in that, in described depressurization steps, temperature is the temperature of more than described polyamide 5X fusing point, is preferably 200 ~ 300 DEG C, is more preferably 230 ~ 260 DEG C.
15. production methods according to any one of claim 10-14, it is characterized in that, in described moisture separating step, temperature is 250 ~ 320 DEG C, is preferably 250 ~ 300 DEG C.
16. production methods according to any one of claim 10-15, it is characterized in that, the temperature of described condensation polymerization step is 250 ~ 320 DEG C, is preferably 250 ~ 300 DEG C; And/or
Described condensation polymerization step is carried out under normal pressure or vacuum condition, adopts inert gas shielding when carrying out polycondensation under normal pressure, and when carrying out polycondensation under vacuum condition, pressure is 0 ~ 760mmHgA, is preferably 150 ~ 250mmHgA.
17. production methods according to any one of claim 10-16, it is characterized in that, described polyamide 5X is polyamide 56.
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| CN110394143A (en) * | 2019-08-21 | 2019-11-01 | 兖州煤业股份有限公司 | A kind of coal resolution tubular type reaction unit |
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