CN115105863B - Liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment and separation method of oil phase in methionine production - Google Patents
Liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment and separation method of oil phase in methionine production Download PDFInfo
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- CN115105863B CN115105863B CN202210473690.7A CN202210473690A CN115105863B CN 115105863 B CN115105863 B CN 115105863B CN 202210473690 A CN202210473690 A CN 202210473690A CN 115105863 B CN115105863 B CN 115105863B
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- 229930182817 methionine Natural products 0.000 title claims abstract description 77
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 title claims abstract description 76
- 239000007788 liquid Substances 0.000 title claims abstract description 60
- 238000000926 separation method Methods 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000007787 solid Substances 0.000 title claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000012071 phase Substances 0.000 claims description 62
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 19
- 230000020477 pH reduction Effects 0.000 claims description 18
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- 235000019253 formic acid Nutrition 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004062 sedimentation Methods 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 11
- 230000008719 thickening Effects 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims description 2
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims 1
- 235000019796 monopotassium phosphate Nutrition 0.000 claims 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims 1
- 235000019799 monosodium phosphate Nutrition 0.000 claims 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims 1
- 239000012452 mother liquor Substances 0.000 abstract description 17
- 238000002425 crystallisation Methods 0.000 abstract description 15
- 230000008025 crystallization Effects 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 14
- 230000009286 beneficial effect Effects 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000701 coagulant Substances 0.000 abstract description 3
- 208000028659 discharge Diseases 0.000 abstract description 3
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 description 16
- 229940091173 hydantoin Drugs 0.000 description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 description 11
- 235000011152 sodium sulphate Nutrition 0.000 description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 10
- 239000000413 hydrolysate Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- CLUWOWRTHNNBBU-UHFFFAOYSA-N 3-methylthiopropanal Chemical compound CSCCC=O CLUWOWRTHNNBBU-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 5
- 150000001413 amino acids Chemical class 0.000 description 5
- 238000000909 electrodialysis Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 description 5
- 235000011181 potassium carbonates Nutrition 0.000 description 5
- 238000007127 saponification reaction Methods 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 4
- 238000013375 chromatographic separation Methods 0.000 description 4
- 150000002741 methionine derivatives Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000011736 potassium bicarbonate Substances 0.000 description 3
- 235000015497 potassium bicarbonate Nutrition 0.000 description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- SBKRXUMXMKBCLD-UHFFFAOYSA-N 5-(2-methylsulfanylethyl)imidazolidine-2,4-dione Chemical compound CSCCC1NC(=O)NC1=O SBKRXUMXMKBCLD-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000009264 composting Methods 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- 235000020776 essential amino acid Nutrition 0.000 description 2
- 239000003797 essential amino acid Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000001360 methionine group Chemical group N[C@@H](CCSC)C(=O)* 0.000 description 2
- 125000002816 methylsulfanyl group Chemical group [H]C([H])([H])S[*] 0.000 description 2
- 239000012982 microporous membrane Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- VWWOJJANXYSACS-UHFFFAOYSA-N 2-hydroxy-4-methylsulfanylbutanenitrile Chemical compound CSCCC(O)C#N VWWOJJANXYSACS-UHFFFAOYSA-N 0.000 description 1
- KKYSBGWCYXYOHA-UHFFFAOYSA-N 3-methylthiopropylamine Chemical compound CSCCCN KKYSBGWCYXYOHA-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 101100425892 Danio rerio tpma gene Proteins 0.000 description 1
- 108010016626 Dipeptides Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 102000007056 Recombinant Fusion Proteins Human genes 0.000 description 1
- 108010008281 Recombinant Fusion Proteins Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 101150048952 TPM-1 gene Proteins 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 1
- 235000019797 dipotassium phosphate Nutrition 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- -1 sodium bicarbonate, hydrocyanic acid derivative Chemical class 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
- B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F7/00—Fertilisers from waste water, sewage sludge, sea slime, ooze or similar masses
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of chemical industry, in particular to liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment and a separation method of an oil phase in methionine production. Compared with the prior art, the method has the advantages that beneficial substances in the impurity enrichment liquid are separated respectively in a way of acidizing crystallization mother liquor which circulates for many times in methionine production, the discharge treatment of the beneficial substances is avoided, lower alcohol or coagulant is not introduced, the separation equipment is simple, the cost is low, the energy consumption is low, and the maximization of the economic environment is realized.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment and a separation method of an oil phase in methionine production.
Background
Methionine, also known as methionine, abbreviated Met, is one of the basic units of a biosynthetic protein and is also an essential amino acid and a limiting amino acid. Met is the only sulfur-containing amino acid in the essential amino acid, and the animal can obviously promote growth by taking a small amount of amino acid, shorten the feeding period, increase the egg and milk yield, and if the intake is insufficient, the utilization of other amino acids in the body is insufficient, the unused amino acid is converted into energy molecules and urea through deamination, and the burden of livers and kidneys is increased. Methionine is widely used in the fields of feed, medicine, food, cosmetics and the like.
The known methionine production process is to synthesize 5- (beta-methylthioethyl) hydantoin, also called hydantoin or hydantoin for short, by using 3-methylthiopropanal, hydrocyanic acid, ammonia and carbon dioxide as raw materials. The hydantoin is hydrolyzed by alkali to obtain hydrolysate of mixture of methionine salt and carbonate. Acidifying the hydrolysate to obtain methionine and filtrate, wherein the filtrate contains a large amount of useful components, and the useful components are required to be recycled after treatment; the difference in acidifying medium and base determines the difference in the return link of the filtrate, which is either returned to the hydrolysis of hydantoin or to the crystallization step.
Hydantoin is an essential intermediate in the mainstream production process of methionine, and alkali such as potassium carbonate, sodium hydroxide, calcium hydroxide, potassium bicarbonate, sodium bicarbonate and the like can be used for hydantoin hydrolysis. The production process of methionine is longer, no matter which alkali is used for hydrolyzing hydantoin, the generation of impurities is unavoidable, and the impurities comprise formic acid, acrolein polymerization derivatives, 3-methylthiopropanal polymerization derivatives, methionine hydroxy analogues, methionine derivative precursors, polycarboxylic acid impurities and the like, and the impurities have similar structures with methionine: or carbon chain or amino or carboxyl, so most of impurities have similar and similar compatible effects with methionine, are difficult to thoroughly separate from methionine, and can lead to reduced quality of extracted methionine and even influence the yield of reaction in the circulating process, so that the separation of impurities is a necessary operation.
The publication CN106748932a uses a microporous membrane filter to remove polymer from a mixed solution of methionine and bicarbonate, and then uses a cation exchange resin to separate the mixture into a methionine solution and a sulfate solution, and uses electrodialysis or stripping and/or an anion exchange resin to separate formic acid from the methionine solution. Firstly, impurities in the crystallization mother liquor are not enriched, and the direct use of cationic resin to change alkaline potassium into neutral potassium is wasteful; second, impurities in the crystallization mother liquor are small molecules and have viscosity, and it is difficult for the microporous membrane filter to filter the impurities and even clog the impurities.
The publication CN102796033B uses an organic solvent to extract the hydrolysate, extracts part of impurities into an organic phase, and the organic phase is distilled and recycled, and the residual liquid is treated as waste liquid. Firstly, methionine salt and carbonate in the saponified solution are high in concentration, and the organic solvent is mixed with part of the saponified solution, so that waste of part of products is caused; second, the organic solvent is partially dissolved in the saponification liquid, resulting in accumulation of the subsequent organic solvent; thirdly, the saponification liquid has low impurity proportion and low extraction efficiency, and part of impurities are basically 3-methylthio propionaldehyde polymer which is not mutually soluble with water, and the TPMA dimer can be controlled to a very low level in the preparation of 5- (2-methylthioethyl) -hydantoin; fourth, the saponification liquid is of strong alkalinity, the carboxyl impurity is more soluble in the water phase, the organic extraction effect is not obvious, but the impurity is one of the main components. The comprehensive organic solvent extraction saponification liquor can only extract a very small amount of impurities in the saponification liquor, and no operation scheme is provided for enrichment of formic acid.
The publication CN110678445a uses electrodialysis to remove anions containing 1 to 5 carbons from the methionine crystallization mother liquor. Electrodialysis does not achieve this well within acceptable times and energy consumption for industrial production; methionine can enter the anolyte due to osmotic pressure or potential difference, and the anolyte still needs further treatment; furthermore, the crystallization mother liquor is enriched in impurities, which may cause blockage of the membrane, and finally lead to poor electrodialysis efficiency or even breakdown.
CN401693082a indicates that methionine produces impurities such as dimethyl disulfide, acrylamide, 3-methylthiopropylamine, etc. during heating, but does not mention heating time, number of times, and temperature. Alkali metal or alkaline earth metal is used in the hydrolysis process of hydantoin, and the mixture of salt and methionine generated by acidification has multiple limitation in the subsequent concentration due to different contents and solubilities of the salt and the methionine, so that the concentration has to be repeated. In order to reduce the number of concentration, methionine practitioners have proposed the following scheme.
In CN107531621A, the hydrolysis liquid is concentrated to extract part of sodium carbonate, and the sodium carbonate returns to the hydrolysis of hydantoin, and then sulfuric acid is used for acidification to extract methionine, so that the consumption of hydrolysis alkaline sodium and sulfuric acid can be reduced, and the generation of sodium sulfate is also reduced. Sodium carbonate is easily dissolved in water, the hydrolysis liquid is concentrated to high multiple and then filtered, the concentration is easy to operate, a large amount of energy is required, and the impurity treatment is not mentioned.
CN104693082a uses chromatographic separation technology to separate sodium sulfate and methionine mixed solution, and CN106432018A uses chromatographic separation technology to separate potassium bicarbonate and methionine mixed solution. The chromatographic separation technology needs to additionally introduce a large amount of water, so that the concentration of methionine solution is low; secondly, the chromatographic separation investment is large, the separation efficiency is low, and most importantly, impurities generated in the methionine preparation are not treated, and the impurities (relative to impurities generated by thermal decomposition) only need to be treated with importance; furthermore, the separation effect of the chromatography on bicarbonate and methionine is considerable.
CN104926701A, CN103772246a uses a resin separation technique to separate the hydrolysate into methionine solution and sodium sulfate solution, and then separately processes to obtain methionine and sodium sulfate. However, because of the solubility problem of methionine and the heat resistance of the ion exchange resin, the saponified solution entering the ion exchange resin column must be diluted to a low concentration, and the subsequent crystallization, concentration and other operation costs are high; the ion exchange resin is also only used for separating sodium sulfate from other components, and intermediates of 3-methylthiopropanal, 2-acrylic acid and acrolein and polymers thereof, formate, methionine dipeptide and pigment enter methionine solution for a great part, and the enrichment of impurities is caused by long-term concentration and crystallization to influence the quality of methionine; the sodium sulfate mother liquor is subjected to evaporative crystallization, so that the impurity enrichment is also caused, and the product quality of sodium sulfate is further influenced; finally, a large amount of water is required to be introduced by using the ion exchange technology, and a large amount of wastewater is generated by subsequent operation, so that the method is unfavorable for environmental protection and economy, and has high cost for the main process flow.
In CN109734637A, CN103922980A, CN103933861A, CN106432020B, CN104130169A, CN103922980A, CN105671587a, a bipolar membrane was used to separate methionine and carbonate/bicarbonate mixed solution into methionine and lye. Firstly, methionine has limited solubility, water is needed to dilute the methionine, and the separated methionine solution needs to be concentrated and crystallized or crystallized at low temperature; secondly, the mixed solution contains a plurality of impurities, which has an influence on the electron utilization efficiency of the bipolar membrane and the service life of the bipolar membrane; thirdly, the bipolar membrane is used for generating low-concentration alkali and still needs to be concentrated for use; fourth, the generated carbon dioxide is neutral molecule, which results in increased solution resistance and low electrodialysis efficiency, and is used in the main process flow with high equipment investment and high operation cost.
Extracting methionine and mother liquor from the hydrolysate in CN1923807A, CN101602700A, CN101602701A, CN110536881A by carbon dioxide acidification, concentrating part of mother liquor, adding lower alcohol to separate a mixture of methionine and potassium carbonate, returning to hydrolysis of hydantoin, and discarding the secondary mother liquor after retreating. The introduction of lower alcohols makes residual recovery of the system problematic.
The impurities, if separated, can maximize the resource benefit of the treatment process other than incineration or biochemistry.
In summary, the treatment can be divided into two ideas of extracting impurities or extracting methionine/salt, because of the greater solubility of methionine and salt in water, the extraction of impurities is not lost as an alternative, however the known published patent still has the following problems:
(1) The treatment of impurities produced in methionine production is not explicitly mentioned;
(2) High-cost and high-energy-consumption equipment technology is used for reducing the separation of methionine and salt by a small part of impurities generated in subsequent treatment;
(3) Treating methionine crystallization mother liquor, and introducing lower alcohol or coagulant;
(4) After methionine crystallization mother liquor is treated, a part of crystallization mother liquor still needs to be discarded, and beneficial substances cannot be recovered;
(5) And the waste of part of crystallization mother liquor is treated into low-value substances by using beneficial resources, so that the cost is increased secondarily.
Disclosure of Invention
In order to solve the problems mentioned in the background art, the invention aims to provide liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment and a separation method of an oil phase in methionine production, which are used for respectively separating beneficial substances from impurity enrichment liquid after methionine is extracted, avoiding discharge treatment of the beneficial substances and solving the subsequent treatment problem of hydantoin hydrolysate.
On the one hand, the invention provides liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment, which is characterized in that: the device comprises a shell, wherein the interior of the shell is divided into a sedimentation zone and a thickening zone from top to bottom, an overflow port is formed in the upper portion of the shell, a solid-liquid separator is connected to a pipeline at the bottom of the shell, and the overflow port, the sedimentation zone and the thickening zone are communicated through a three-phase separator. In actual operation, the acidizing fluid is separated in a flowing way between a sedimentation zone and a thickening zone through a three-phase separator, the oil phase at the upper layer of the sedimentation zone flows out from an overflow port, and the acid-containing aqueous solution and the solid mixture in the thickening zone are separated through a solid-liquid separator.
Preferably, the three-phase separator comprises a bypass pipe and a plurality of inclined pipes, wherein the bypass pipe and the inclined pipes are vertically arranged, the upper end and the lower end of the bypass pipe are respectively communicated with the overflow port and the dense area, the upper end and the lower end of the inclined pipes are respectively communicated with the bypass pipe and the sedimentation area, a plurality of inclined plates are arranged in parallel in the sedimentation area from top to bottom, and each inclined plate is correspondingly arranged above the outlet of the inclined pipe one by one. In actual operation, the inclined tube can reduce the flowing stress of liquid, two liquid phases with different densities are automatically transferred into the bypass tube for further separation, the oil phase flows out from the overflow port, the acid-containing aqueous solution with high density and a small amount of solid are naturally settled to a dense area, and the continuous separation of liquid-liquid two phases or liquid-solid three phases is realized.
Preferably, the feed inlet of the solid-liquid separator is communicated with the bottom of the thickening area, and the liquid outlet of the solid-liquid separator is communicated with the upper part of the thickening area. In actual operation, in order to ensure the liquid level of the upper layer, the oil phase can overflow out, and part of separated liquid is refluxed to the dense area.
On the other hand, the separation method of the oil phase in methionine production is characterized by comprising the following steps:
s1, adding acid into the impurity enrichment solution for acidification until the pH value of the acidification solution is less than 4;
s2, distilling the acidizing fluid at 60-100 ℃ to remove formic acid;
s3, separating the acidification liquid from which the formic acid is removed into an oil phase, a water phase and a solid phase by using the equipment. In actual operation, mother liquor recycled for many times in methionine production is used as impurity enrichment liquid, and the impurity enrichment liquid contains one or more of the following components except solvent water: methionine, methionine derivative, 3-methylthio propionaldehyde and polymer and derivative, potassium carbonate, potassium bicarbonate, potassium hydroxide, sodium sulfate, sodium carbonate, sodium bicarbonate, hydrocyanic acid derivative hydrolysate and hydrocyanic acid hydrolysate formic acid, because most of impurities generated in methionine production contain carboxyl, after enrichment in the system, layering can occur with the system by adjusting pH, the upper layer is a red-black oil phase, the lower layer is a system aqueous solution, oil phase impurities are thoroughly adsorbed on other impurities, even the aqueous solution is changed from original black red to light yellow, methionine is changed into methionine acid salt under an acid system, and the methionine has extremely high solubility in water, so that oil phase impurities are thoroughly/thoroughly separated.
Preferably, the acid in S1 is one or more of hydrochloric acid, phosphoric acid, sulfuric acid, sodium bisulfate, potassium bisulfate, ammonium bisulfate, sodium hydrogen phosphate, disodium hydrogen phosphate, potassium hydrogen phosphate, dipotassium hydrogen phosphate and ammonium hydrogen phosphate.
Preferably, the pH of the acidizing fluid in S1 is less than 3. In practical operation, as formic acid is dissolved in both the aqueous phase and the organic phase, formate in the acidified liquid is changed into formic acid for removal, and the organic phase and the aqueous phase are separated more thoroughly and rapidly.
Preferably, S2 is specifically: extracting the acidizing fluid by using steam and circulating gas at 60-100 ℃ for 10-100min, and returning the gas phase containing formic acid into the acidizing fluid after absorbing the gas phase by alkali liquor. In actual operation, after cyclic extraction, the alkali liquor can be concentrated to prepare formate, the concentrated water can be used for supplementing water in the acidizing fluid, and the pH value of the acidizing fluid can be stabilized to a certain value.
Preferably, the recycle gas is carbon dioxide gas.
Preferably, the alkali liquor is prepared by dissolving one or more of alkali metal and alkaline earth metal oxides, hydroxides and carbonates in water.
Preferably, in S3, the acidizing fluid is introduced into a separation device, the temperature is controlled to be 30-80 ℃, continuous liquid-liquid or liquid-solid separation is carried out, the upper layer of a sedimentation zone of the separation device is oil phase impurities, the middle layer is acid-containing aqueous solution, and the lower layer is solid. In practical operation, the temperature of the acidizing fluid needs to be controlled, and the pH value of the overflowed oil phase is adjusted to 5-7, so that the fluidity of oil phase impurities can be increased, and the oily impurities mainly comprise 2-hydroxy-4-methylthiobutyronitrile, 3-methylthiopropanal, polymers and polymer hydrolysates and hydrolysates of hydrocyanic acid, water, potassium sulfate and the like.
The beneficial effects are that: compared with the prior art, the method has the advantages that beneficial substances in the impurity enrichment liquid are separated respectively in a way of acidizing crystallization mother liquor which circulates for many times in methionine production, the discharge treatment of the beneficial substances is avoided, lower alcohol or coagulant is not introduced, the separation equipment is simple, the cost is low, the energy consumption is low, and the maximization of the economic environment is realized.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The present invention is described in detail below by way of specific examples, which are given herein for the purpose of further illustration only and are not to be construed as limiting the scope of the present invention, as many insubstantial modifications and variations of the present invention will become apparent to those skilled in the art in light of the foregoing disclosure. Except for special descriptions, the parts are parts by weight, the percentages are mass percentages, and the concentrations are mass percentage concentrations.
Example 1
The utility model provides a continuous separation equipment of liquid-liquid two-phase or liquid-liquid solid three-phase, includes casing 1, the inside of casing 1 is from last subsidence area a and the dense zone b of dividing into down, overflow mouth 2 has been seted up on the upper portion of casing 1, casing 1 bottom pipe connection has solid-liquid separator 3, overflow mouth 2 subsidence area a with communicate through the three-phase separator between the dense zone b.
Example 2
The continuous separation equipment for liquid-liquid two phases or liquid-solid three phases comprises a machine shell 1, wherein the interior of the machine shell 1 is divided into a sedimentation zone a and a dense zone b from top to bottom, an overflow port 2 is formed in the upper portion of the machine shell 1, a solid-liquid separator 3 is connected to the bottom of the machine shell 1 through a pipeline, a feed inlet of the solid-liquid separator 3 is communicated with the bottom of the dense zone b, a liquid outlet of the solid-liquid separator 3 is communicated with the upper portion of the dense zone b, and the overflow port 2, the sedimentation zone a and the dense zone b are communicated through a three-phase separator; the three-phase separator comprises a bypass pipe 4 and a plurality of inclined pipes 5 which are vertically arranged, wherein the upper end and the lower end of the bypass pipe 4 are respectively communicated with the overflow port 2 and the thickening area b, the upper end and the lower end of the inclined pipes 5 are respectively communicated with the bypass pipe 4 and the sedimentation area a, a plurality of inclined plates 6 are arranged in parallel in the sedimentation area a from top to bottom, and each inclined plate 6 is arranged above the outlet of the inclined pipe 5 in a one-to-one correspondence manner.
Example 3
The apparatus of example 2 was used for separation of oil phase in the production of isolated methionine.
The impurity enrichment liquid source is concentrated solution obtained by extracting methionine through sulfuric acid acidification and concentrating sodium sulfate extraction of sodium hydroxide hydrolysate of hydantoin or mother solution obtained by repeatedly extracting methionine and sodium sulfate for impurity enrichment for many times in the process of hydrolyzing hydantoin by sodium hydroxide, wherein the methionine content is 0.5-3wt%, the formate content is 1-5wt%, the sodium sulfate content is 10-30wt% and the methylthio impurity content is 1-10wt%.
The pH value of the impurity enrichment liquid is adjusted to 2.4 by sulfuric acid, formic acid is removed from the acidification liquid by using carbon dioxide/steam at 60-100 ℃, the removal gas is absorbed by alkali liquor and then returns to carry out gas stripping on the acidification liquid, the formic acid is removed for 40-60min, when the pH value of the acidification liquid is stabilized to 2.7, the acidification liquid is continuously transferred into separation equipment, the temperature of materials in the separation equipment is controlled to be 35-45 ℃, the pH value of overflowed oil phase substances is adjusted to 5-7 by using ammonia, and the oil phase substances comprise N, S at the moment, so that the method is particularly suitable for composting.
Example 4
The apparatus of example 2 was used for separation of oil phase in the production of isolated methionine.
The source of the impurity enrichment liquid is crystallization mother liquor for extracting methionine by carbon dioxide acidification of potassium carbonate hydrolysate of hydantoin in the process of hydrolyzing hydantoin by potassium carbonate or mother liquor for extracting methionine to be enriched by impurities by repeatedly regenerating hydrolyzed hydantoin and extracting methionine, wherein the methionine content is 0.5-3wt%, the formate content is 1-5wt%, the alkaline potassium content is 0.2-2wt% and the methylthio impurity content is 1-10wt%.
The pH value of the impurity enrichment liquid is adjusted to 2.2 by sulfuric acid, formic acid is removed from the acidification liquid by using carbon dioxide/steam at 60-100 ℃, the removal gas is returned to carry out gas stripping on the acidification liquid after being absorbed by alkali liquor, the formic acid is removed for 10-30min, when the pH value of the acidification liquid is stabilized to 2.4, the acidification liquid is continuously transferred into separation equipment, the material temperature in the separation equipment is controlled to be 30-60 ℃, the pH value of overflowed oil phase substances is adjusted to 5-7 by using ammonia, and the oil phase substances comprise N, S, K at the moment and are particularly suitable for composting.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (7)
1. A method for separating an oil phase in methionine production, comprising the steps of:
s1, adding acid into the impurity enrichment solution for acidification until the pH value of the acidification solution is less than 4;
s2, distilling the acidizing fluid at 60-100 ℃ to remove formic acid;
s3, separating the acidulated liquid from which the formic acid is removed into an oil phase, a water phase and a solid phase by using liquid-liquid two-phase or liquid-solid three-phase continuous separation equipment;
the liquid-liquid two-phase or liquid-solid three-phase continuous separation device comprises a shell (1), wherein the interior of the shell (1) is divided into a sedimentation zone (a) and a thickening zone (b) from top to bottom, an overflow port (2) is formed in the upper part of the shell (1), a solid-liquid separator (3) is connected to a pipeline at the bottom of the shell (1), and the overflow port (2), the sedimentation zone (a) and the thickening zone (b) are communicated through a three-phase separator;
the three-phase separator comprises a bypass pipe (4) and a plurality of inclined pipes (5) which are vertically arranged, wherein the upper end and the lower end of the bypass pipe (4) are respectively communicated with the overflow port (2) and the thickening area (b), the upper end and the lower end of the inclined pipe (5) are respectively communicated with the bypass pipe (4) and the sedimentation area (a), a plurality of inclined plates (6) are arranged in parallel from top to bottom in the sedimentation area (a), and each inclined plate (6) is arranged above the outlet of the inclined pipe (5) in a one-to-one correspondence manner; the feed inlet of the solid-liquid separator (3) is communicated with the bottom of the dense zone (b), and the liquid outlet of the solid-liquid separator (3) is communicated with the upper part of the dense zone (b).
2. The method for separating an oil phase in methionine production according to claim 1, wherein: the acid in S1 is one or more of hydrochloric acid, phosphoric acid, sulfuric acid, sodium bisulfate, potassium bisulfate, ammonium bisulfate, sodium dihydrogen phosphate, disodium hydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate and ammonium hydrogen phosphate.
3. The method for separating an oil phase in methionine production according to claim 1, wherein: in S1, pH of the acidizing fluid is less than 3.
4. The method for separating oil phase in methionine production according to claim 1, wherein S2 is specifically: extracting the acidizing fluid by using steam and circulating gas at the temperature of 60-100 ℃ for 10-100min, and returning the gas phase containing formic acid into the acidizing fluid after absorbing the gas phase by alkali liquor.
5. The method for separating an oil phase in methionine production according to claim 4, wherein: the circulating gas is carbon dioxide gas.
6. The method for separating an oil phase in methionine production according to claim 4, wherein the alkali liquid is one or more of alkali metal and alkaline earth metal oxides, hydroxides, carbonates, and is prepared by dissolving in water.
7. The method for separating an oil phase in methionine production according to claim 1, wherein in S3, the acidified liquid is introduced into a separating device, the temperature is controlled to be 30-80 ℃, and continuous liquid-liquid or liquid-solid separation is performed, wherein the upper layer of a settling zone of the separating device is oil phase impurities, the middle layer is an acid-containing aqueous solution, and the lower layer is solid.
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| US8337706B2 (en) * | 2007-10-14 | 2012-12-25 | 1612017 Alberta Ltd. | Solids removal system and method |
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| CN206142879U (en) * | 2016-09-10 | 2017-05-03 | 盘锦金宇众和工程服务有限公司 | Oil field filter -pressing water oil -water separator |
| CN106512491A (en) * | 2017-01-23 | 2017-03-22 | 太原市润民环保节能有限公司 | Turnover precipitation separation device |
| CN211383924U (en) * | 2019-08-14 | 2020-09-01 | 上海洗霸科技股份有限公司 | Double-layer filler precipitation device |
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