CN104910052A - System for preparing 2-amidogen-1-naphthalene sulfonic acid - Google Patents
System for preparing 2-amidogen-1-naphthalene sulfonic acid Download PDFInfo
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- CN104910052A CN104910052A CN201510391786.9A CN201510391786A CN104910052A CN 104910052 A CN104910052 A CN 104910052A CN 201510391786 A CN201510391786 A CN 201510391786A CN 104910052 A CN104910052 A CN 104910052A
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 151
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 238000003860 storage Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 19
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 19
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 17
- 238000004821 distillation Methods 0.000 claims abstract description 15
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 14
- 238000005194 fractionation Methods 0.000 claims abstract description 14
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 12
- 238000006482 condensation reaction Methods 0.000 claims abstract description 11
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 9
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 8
- 230000020477 pH reduction Effects 0.000 claims description 12
- PJKVFARRVXDXAD-UHFFFAOYSA-N 2-naphthaldehyde Chemical compound C1=CC=CC2=CC(C=O)=CC=C21 PJKVFARRVXDXAD-UHFFFAOYSA-N 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 abstract 6
- 229950011260 betanaphthol Drugs 0.000 abstract 3
- 238000001556 precipitation Methods 0.000 abstract 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- GWIAAIUASRVOIA-UHFFFAOYSA-N 2-aminonaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(N)=CC=C21 GWIAAIUASRVOIA-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 150000005004 2-naphthylamines Chemical class 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000006396 nitration reaction Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- HDFQKJQEWGVKCQ-UHFFFAOYSA-N 1,3-dimethyl-2-nitrobenzene Chemical class CC1=CC=CC(C)=C1[N+]([O-])=O HDFQKJQEWGVKCQ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004176 ammonification Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- XTHPWXDJESJLNJ-UHFFFAOYSA-N sulfurochloridic acid Chemical compound OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- PXWYZLWEKCMTEZ-UHFFFAOYSA-N 1-ethyl-2-nitrobenzene Chemical compound CCC1=CC=CC=C1[N+]([O-])=O PXWYZLWEKCMTEZ-UHFFFAOYSA-N 0.000 description 1
- SQAINHDHICKHLX-UHFFFAOYSA-N 1-naphthaldehyde Chemical compound C1=CC=C2C(C=O)=CC=CC2=C1 SQAINHDHICKHLX-UHFFFAOYSA-N 0.000 description 1
- BBUPBICWUURTNP-UHFFFAOYSA-N 2,4-dimethyl-1-nitrobenzene Chemical compound CC1=CC=C([N+]([O-])=O)C(C)=C1 BBUPBICWUURTNP-UHFFFAOYSA-N 0.000 description 1
- SGBQUMZTGSQNAO-UHFFFAOYSA-N 2-hydroxynaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(O)=CC=C21 SGBQUMZTGSQNAO-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 150000005002 naphthylamines Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a system for preparing 2-amidogen-1-naphthalene sulfonic acid. The system comprises a raw material reaction tower, a first separation reaction tower, a condensation reaction tower, a temperature division reaction tower, a precipitation reaction tower, a fractionation reaction tower, a first synthetic reaction tower, a neutralization reaction tower, a second separation reaction tower, a distillation reaction tower, a second synthetic reaction tower, an acidizing reaction tower, a dehydration reaction tower, a waste water treatment system, a hydrogen chloride gas storage bottle, a hydrogen chloride liquid storage tank, an ammonia gas storage bottle, an ammonium sulfate liquid storage tank, a sodium sulfate liquid storage tank, a 2-naphthol storage tank, a finished product storage tank and an m-xylene storage tank. Raw materials include dry hydrogen chloride gas, m-xylene and 2-naphthol. Product purity is high and more than 96.3%, the total amino value of powder from white to light pink (according to dry products) is higher than 98.5%, the content of the 2-naphthol is lower than 0.01%, the content of water is lower than 1.0%, and the content of an isomer is smaller than 1%.
Description
Technical field
The present invention relates to a kind of system preparing 2-amino-1-naphthalene sulfonic aicd, belong to chemical field.
Background technology
TOBIAS ACID 97MIN.& 98MIN. chemical name 2-amino-1-naphthalene sulfonic aicd.TOBIAS ACID 97MIN.& 98MIN. synthesis system is take beta naphthal as raw material, beta naphthal in o-nitroethylbenzene solution using chlorsulfonic acid as sulphonating agent, sulfonation first generates 2-tea phenol-1-sulfonic acid, oxy-Tobias acid sodium is obtained with being separated with in alkali, again by ammoniacal liquor ammonia solution under acidic bisulfite is by existence, obtain 2-naphthylamines-1-sodium sulfonate, with hcl acidifying, filtering separation obtains TOBIAS ACID 97MIN.& 98MIN..Due in production system, so easily there is side reaction during ammonification in the impossible complete reaction of raw material beta naphthal.Simultaneously because sulfonic group generating portion hydrolysis in TOBIAS ACID 97MIN.& 98MIN. molecule comes off, make in Industrial products containing a certain amount of severe toxicity and strongly carcinogenic 2-naphthylamines impurity.Domestic and international many scholars have done much research and probe work in the content reducing 2-naphthylamines, mainly comprise: the change of (1) system condition, proportioning; (2) utilize nitrobenzene extraction sulfonated products, extract aminate with toluene; (3) the 2-naphthylamines in TOBIAS ACID 97MIN.& 98MIN. is removed with sorbent materials such as gacs.
TOBIAS ACID 97MIN.& 98MIN. waste liquor be a kind of brownish, organic concentration is high, main organic composition in the acid waste water waste liquor of strong toxicity, difficult for biological degradation has TOBIAS ACID 97MIN.& 98MIN., through base TOBIAS ACID 97MIN.& 98MIN. and a naphthylamines etc. from the above, except containing except a large amount of inorganic salt in TOBIAS ACID 97MIN.& 98MIN. waste liquor, also can be reclaimed the organism in waste water by the method for crystallisation by cooling or the dark contracting of evaporation containing a large amount of organism inorganic salt, although its concentration is very large, directly can't makes raw materials for production and use and must first concentrate.
Summary of the invention
For prior art Problems existing, the invention provides a kind of system preparing 2-amino-1-naphthalene sulfonic aicd, this system comprises raw material reaction tower, first separating reaction tower, condensation reaction tower, divide warm reaction tower, precipitin reaction tower, fractionation reaction tower, first building-up reactions tower, neutralization reaction tower, second separating reaction tower, distillation reaction tower, second building-up reactions tower, acidification reaction tower, dehydration reaction tower, Waste Water Treatment, hydrogen chloride gas storage bottle, hydrogen chloride liquid hold-up vessel, ammonia gas storage bottle, ammonium sulfate liquid hold-up vessel, sodium sulfate liquid storage tank, beta naphthal hold-up vessel, product storage tank, m-xylene hold-up vessel, wherein, the air outlet of hydrogen chloride gas storage bottle connects the air intake of raw material reaction tower by pipeline, the discharge port of raw material reaction tower connects the feeding mouth of the first separating reaction tower by pipeline, the discharge port of the first separating reaction tower connects the feeding mouth of condensation reaction tower by pipeline, the discharge port of condensation reaction tower connects the first feeding mouth of the first building-up reactions tower by pipeline, the discharge port of m-xylene hold-up vessel connects the feeding mouth of point warm reaction tower by pipeline, the discharge port of warm reaction tower is divided to connect the feeding mouth of precipitin reaction tower by pipeline, the discharge port of precipitin reaction tower connects the feeding mouth of fractionation reaction tower by pipeline, the feeding mouth of fractionation reaction tower connects the 3rd feeding mouth of the first building-up reactions tower by pipeline, the discharge port of beta naphthal hold-up vessel connects the first building-up reactions tower second feeding mouth by pipeline, the discharge port of the first building-up reactions tower connects the feeding mouth of neutralization reaction tower by pipeline, the discharge port of neutralization reaction tower connects the feeding mouth of the second separating reaction tower by pipeline, the discharge port of the second separating reaction tower connects the feeding mouth of distillation reaction tower by pipeline, the discharge port of distillation reaction tower connects the feeding mouth of the second building-up reactions tower by pipeline, the discharge port of the second building-up reactions tower connects the feeding mouth of acidification reaction tower by pipeline, the discharge port of acidification reaction tower connects the feeding mouth of dehydration reaction tower by pipeline, the discharge port of dehydration reaction tower connects the feeding mouth of product storage tank by pipeline, the water port of fractionation reaction tower connects the first water inlet of Waste Water Treatment by pipeline, the water port of the second separating reaction tower connects the second water inlet of Waste Water Treatment by pipeline, the water port of distillation reaction tower connects the 3rd water inlet of Waste Water Treatment by pipeline, the water port of dehydration reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline, the liquid outlet of hydrogen chloride liquid hold-up vessel connects the fluid inlet of acidification reaction tower by pipeline, the air outlet of ammonia gas storage bottle connects the inlet mouth of the second building-up reactions tower by pipeline, the liquid outlet of ammonium sulfate liquid hold-up vessel connects the fluid inlet of the second building-up reactions tower by pipeline, the liquid outlet of sodium sulfate liquid storage tank connects the fluid inlet of neutralization reaction tower by pipeline.
The ingress of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
In point warm reaction tower respectively 0-15 DEG C, 15-17 DEG C, 17-25 DEG C, to react at 25-30 DEG C.
The invention has the advantages that:
(1) production and improvement come into operation simultaneously, and production energy consumption is low, and product production is high, and reduce production cost, whole process needs automatization without the need to manual operation.
(2) the 2-amino-1-naphthalene sulfonic aicd product purity prepared by native system is high, and more than 96.3%, white is to baby pink powder, total amido value (in dry product) is more than 98.5%, 2-naphthylamines content is below 0.01%, and water content is lower than 1.0%, and content of isomer is less than 1%.
(3) to the transformation and upgrade of original technology, have employed emerging raw material and produce, reaction efficiency is high, with short production cycle, has good market outlook.
Accompanying drawing explanation
Fig. 1 is the system schematic of preparation 2-amino-1-naphthalene sulfonic aicd.
In figure: 1-raw material reaction tower, 2-first separating reaction tower, 3-condensation reaction tower, 4-divides warm reaction tower, 5-precipitin reaction tower, 6-fractionation reaction tower, 7-first building-up reactions tower, 8-neutralization reaction tower, 9-second separating reaction tower, 10-distillation reaction tower, 11-second building-up reactions tower, 12-acidification reaction tower, 13-dehydration reaction tower, 14-Waste Water Treatment, 15-hydrogen chloride gas storage bottle, 16-hydrogen chloride liquid hold-up vessel, 17-ammonia gas storage bottle, 18-ammonium sulfate liquid hold-up vessel, 19-sodium sulfate liquid storage tank, 20-beta naphthal hold-up vessel, 21-product storage tank, 22-m-xylene hold-up vessel.
Embodiment
A kind of system preparing 2-amino-1-naphthalene sulfonic aicd as shown in Figure 1, this system comprises raw material reaction tower 1, first separating reaction tower 2, condensation reaction tower 3, divide warm reaction tower 4, precipitin reaction tower 5, fractionation reaction tower 6, first building-up reactions tower 7, neutralization reaction tower 8, second separating reaction tower 9, distillation reaction tower 10, second building-up reactions tower 11, acidification reaction tower 12, dehydration reaction tower 13, Waste Water Treatment 14, hydrogen chloride gas storage bottle 15, hydrogen chloride liquid hold-up vessel 16, ammonia gas storage bottle 17, ammonium sulfate liquid hold-up vessel 18, sodium sulfate liquid storage tank 19, beta naphthal hold-up vessel 20, product storage tank 21, m-xylene hold-up vessel 22, wherein, the air intake 1,25 DEG C that the air outlet of hydrogen chloride gas storage bottle 15 connects raw material reaction tower by pipeline passes in the dry incoming stock reaction tower 1 of hydrogen chloride gas, and the vitriol oil in tower and sulfur trioxide gas react.The discharge port of raw material reaction tower 1 connects the feeding mouth of the first separating reaction tower 2 by pipeline, produce water smoke in knockout tower, absorbs the HSO generated
3cl.The discharge port of the first separating reaction tower 2 connects the feeding mouth of condensation reaction tower 3 by pipeline, lower the temperature, by gaseous state HSO in tower
3cl becomes liquid state, discharges impurity waste gas simultaneously.The discharge port of condensation reaction tower 3 connects the first feeding mouth of the first building-up reactions tower 7 by pipeline, liquid HSO3Cl raw material and other two kinds of raw materials enter in tower and react.The discharge port of m-xylene hold-up vessel 22 connects the feeding mouth of point warm reaction tower 4 by pipeline, raw material m-xylene is added in point warm reaction tower 4 by pipeline.M-xylene, in point warm reaction tower, is first cooled to 0-15 DEG C, adds cooled nitration mixture (56.5% sulfuric acid, 28% nitric acid, 15.5% water), react 1 hour; Intensification after question response completes, maintains the temperature at 15-17 DEG C, adds nitration mixture, reacts 3 hours; Intensification after question response completes, maintains the temperature at 17-25 DEG C, reacts 2 hours; Intensification after question response completes, maintains the temperature at 25-30 DEG C, adds nitration mixture, the 1 little time-division of reaction, and the discharge port of warm reaction tower 4 connects the feeding mouth of precipitin reaction tower 5 by pipeline.Discharging in point warm reaction tower 4 is in precipitin reaction tower 5, and 25-30 DEG C are stirred 30min, leave standstill 5 hours, after liquid material layering, are separated by upper strata itrated compound, adds and is washed to till congo-red test paper shows acidity.The discharging of precipitin reaction tower 5 flows into the feeding mouth of fractionation reaction tower 6 by pipeline, distill in tower, collect 78-85 DEG C of (667Pa) cuts, freezing and crystallizing afterwards, obtains 2,6 dimethyl nitrobenzenes, by-product 2,4 dimethyl nitrobenzene simultaneously.The feeding mouth of fractionation reaction tower 6 connects the 3rd feeding mouth of the first building-up reactions tower 7 by pipeline, 2,6 dimethyl nitrobenzenes and other two kinds of raw materials add in the first building-up reactions tower 7.The discharge port of beta naphthal hold-up vessel 20 connects the first building-up reactions tower 7 second feeding mouth by pipeline, adds in the first building-up reactions tower 7 with other two kinds of raw materials simultaneously.The discharge port of the first building-up reactions tower 7 connects the feeding mouth of neutralization reaction tower 8 by pipeline, in tower, sulfonation reaction occurs, and throws the beta naphthal measured, and continue cooling in tower when stirring, and when in tower, temperature is down to 15 DEG C, starts toward Ta Neijia chlorsulfonic acid.The acid adding period is about 30 minutes, adds rear maintenance 2 hours.The discharge port of neutralization reaction tower 8 connects the feeding mouth of the second separating reaction tower 9 by pipeline, after monitoring device, add a water to scale, when stirring, throwing sodium sulfate, open material feeding valve and enter sulfonated bodies, control ph during charging in tower.The discharge port of the second separating reaction tower 9 connects the feeding mouth of distillation reaction tower 10 by pipeline, be drawn onto in distillation reaction tower 10 after leaving standstill certain hour by lower floor's sodium salt, to be separated complete.The discharge port of distillation reaction tower 10 connects the feeding mouth of the second building-up reactions tower 11 by pipeline.The discharge port of the second building-up reactions tower 11 connects the feeding mouth of acidification reaction tower 12 by pipeline, aminating reaction is there is in tower, the ammoniumsulphate soln measured from ammonium sulfate scale tank toward Ta Neijia, then starts, into qualified corrective sodium salt, accurately to measure volume of material after material feeding, start and stir, close all valves on tower, pot inner pressure is raised to certain pressure, and temperature is 90 DEG C, keep 4 hours at this temperature, ammonification terminates.The discharge port of acidification reaction tower 12 connects the feeding mouth of dehydration 13 reaction tower by pipeline, to the water that Ta Neijia is certain, after complete material, start toward Ta Neijia hydrochloric acid, acid addition time controls at 20 ~ 30 minutes and control ph, after adding acid, but to keep in tower being negative pressure, blow and catch up with that the qualified rear beginning of sulfurous gas is centrifugal to get product.The discharge port of dehydration reaction tower 13 connects the feeding mouth of product storage tank 21 by pipeline, check mechanical, electrical, whether instrument normally handy, whether filter bag intact, open discharging bottom valve, starter motor, adjusting rotary speed, after whizzer works well, drive feed valve, start centrifugal, dispensing speed is wanted evenly, can not be too fast, when being fed to specified rate in rotary drum, close feed valve, adjusting rotary speed, at a high speed, dewaters complete, adjusting rotary speed, to low speed, can play material after whizzer stops operating.The water port of fractionation reaction tower 6 connects the first water inlet of wastewater treatment 14 system by pipeline, the water port of the second separating reaction tower 9 connects the second water inlet of Waste Water Treatment 14 by pipeline, the water port of distillation reaction tower 10 connects the 3rd water inlet of Waste Water Treatment 14 by pipeline, the water port of dehydration reaction tower 13 connects the 4th water inlet of Waste Water Treatment 14 by pipeline, the liquid outlet of hydrogen chloride liquid hold-up vessel 16 connects the fluid inlet of acidification reaction tower 12 by pipeline, when reaction starts in tower, in tower, pass into hydrogen chloride liquid.The air outlet of ammonia gas storage bottle 17 connects the inlet mouth of the second building-up reactions tower 11 by pipeline, when aminating reaction starts, in tower, pass into ammonia.The liquid outlet of ammonium sulfate liquid hold-up vessel 18 connects the fluid inlet of the second building-up reactions tower 11 by pipeline, the liquid outlet of sodium sulfate liquid storage tank 19 connects the fluid inlet of neutralization reaction tower 8 by pipeline.
Claims (3)
1. prepare the system of 2-amino-1-naphthalene sulfonic aicd for one kind, it is characterized in that, this system comprises raw material reaction tower, first separating reaction tower, condensation reaction tower, divide warm reaction tower, precipitin reaction tower, fractionation reaction tower, first building-up reactions tower, neutralization reaction tower, second separating reaction tower, distillation reaction tower, second building-up reactions tower, acidification reaction tower, dehydration reaction tower, Waste Water Treatment, hydrogen chloride gas storage bottle, hydrogen chloride liquid hold-up vessel, ammonia gas storage bottle, ammonium sulfate liquid hold-up vessel, sodium sulfate liquid storage tank, beta naphthal hold-up vessel, product storage tank, m-xylene hold-up vessel etc., wherein, the air outlet of hydrogen chloride gas storage bottle connects the air intake of raw material reaction tower by pipeline, the discharge port of raw material reaction tower connects the feeding mouth of the first separating reaction tower by pipeline, the discharge port of the first separating reaction tower connects the feeding mouth of condensation reaction tower by pipeline, the discharge port of condensation reaction tower connects the first feeding mouth of the first building-up reactions tower by pipeline, the discharge port of m-xylene hold-up vessel connects the feeding mouth of point warm reaction tower by pipeline, the discharge port of warm reaction tower is divided to connect the feeding mouth of precipitin reaction tower by pipeline, the discharge port of precipitin reaction tower connects the feeding mouth of fractionation reaction tower by pipeline, the feeding mouth of fractionation reaction tower connects the 3rd feeding mouth of the first building-up reactions tower by pipeline, the discharge port of beta naphthal hold-up vessel connects the first building-up reactions tower second feeding mouth by pipeline, the discharge port of the first building-up reactions tower connects the feeding mouth of neutralization reaction tower by pipeline, the discharge port of neutralization reaction tower connects the feeding mouth of the second separating reaction tower by pipeline, the discharge port of the second separating reaction tower connects the feeding mouth of distillation reaction tower by pipeline, the discharge port of distillation reaction tower connects the feeding mouth of the second building-up reactions tower by pipeline, the discharge port of the second building-up reactions tower connects the feeding mouth of acidification reaction tower by pipeline, the discharge port of acidification reaction tower connects the feeding mouth of dehydration reaction tower by pipeline, the discharge port of dehydration reaction tower connects the feeding mouth of product storage tank by pipeline, the water port of fractionation reaction tower connects the first water inlet of Waste Water Treatment by pipeline, the water port of the second separating reaction tower connects the second water inlet of Waste Water Treatment by pipeline, the water port of distillation reaction tower connects the 3rd water inlet of Waste Water Treatment by pipeline, the water port of dehydration reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline, the liquid outlet of hydrogen chloride liquid hold-up vessel connects the fluid inlet of acidification reaction tower by pipeline, the air outlet of ammonia gas storage bottle connects the inlet mouth of the second building-up reactions tower by pipeline, the liquid outlet of ammonium sulfate liquid hold-up vessel connects the fluid inlet of the second building-up reactions tower by pipeline, the liquid outlet of sodium sulfate liquid storage tank connects the fluid inlet of neutralization reaction tower by pipeline.
2. the system of preparation 2-amino-1-naphthalene sulfonic aicd according to claim 1, it is characterized in that, the ingress of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
3. the system of preparation 2-amino-1-naphthalene sulfonic aicd according to claim 1, is characterized in that, in point warm reaction tower respectively 0-15 DEG C, 15-17 DEG C, 17-25 DEG C, to react at 25-30 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510391786.9A CN104910052B (en) | 2015-07-07 | 2015-07-07 | System for preparing 2-amidogen-1-naphthalene sulfonic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935893A (en) * | 2017-10-26 | 2018-04-20 | 青岛海湾集团有限公司 | A kind of production line for producing a variety of dyestuff intermediates |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2073746A (en) * | 1980-03-18 | 1981-10-21 | Sumitomo Chemical Co | Process for Producing Mono Alkali Salt of 1-Amino-8-naphthol- 3,6-disulfonic Acid |
| CN101811998A (en) * | 2010-05-17 | 2010-08-25 | 天津大学 | Preparation method of 1-amino-2-naphthol-4-sulfonic acid |
| CN104725282A (en) * | 2014-07-17 | 2015-06-24 | 叶良梅 | Novel environment-friendly production process of 1-naphthol-4-sulfonic acid |
| CN204752572U (en) * | 2015-07-07 | 2015-11-11 | 金双蕾 | System for preparation 2 - amino - 1 - naphthalenesulfonic acid |
-
2015
- 2015-07-07 CN CN201510391786.9A patent/CN104910052B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2073746A (en) * | 1980-03-18 | 1981-10-21 | Sumitomo Chemical Co | Process for Producing Mono Alkali Salt of 1-Amino-8-naphthol- 3,6-disulfonic Acid |
| CN101811998A (en) * | 2010-05-17 | 2010-08-25 | 天津大学 | Preparation method of 1-amino-2-naphthol-4-sulfonic acid |
| CN104725282A (en) * | 2014-07-17 | 2015-06-24 | 叶良梅 | Novel environment-friendly production process of 1-naphthol-4-sulfonic acid |
| CN204752572U (en) * | 2015-07-07 | 2015-11-11 | 金双蕾 | System for preparation 2 - amino - 1 - naphthalenesulfonic acid |
Non-Patent Citations (1)
| Title |
|---|
| 张天永等: ""溶剂法合成1-氨基-4-萘磺酸钠方法的改进"", 《精细化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935893A (en) * | 2017-10-26 | 2018-04-20 | 青岛海湾集团有限公司 | A kind of production line for producing a variety of dyestuff intermediates |
| CN107935893B (en) * | 2017-10-26 | 2020-05-22 | 青岛海湾集团有限公司 | Production line capable of producing various dye intermediates |
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