CN204752566U - Production system of industry preparation 2 - carboxyl - 3 - naphthoic acid - Google Patents

Production system of industry preparation 2 - carboxyl - 3 - naphthoic acid Download PDF

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Publication number
CN204752566U
CN204752566U CN201520390917.7U CN201520390917U CN204752566U CN 204752566 U CN204752566 U CN 204752566U CN 201520390917 U CN201520390917 U CN 201520390917U CN 204752566 U CN204752566 U CN 204752566U
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reaction tower
pipeline
connects
feeding mouth
discharge port
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CN201520390917.7U
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李宇钟
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Abstract

The utility model provides a production system of industry preparation 2 - carboxyl - 3 - naphthoic acid (b), (b) this system include that initial response tower, carboxylation reaction tower, second reaction tower, neutralization reaction tower, acid out reaction tower, filter -pressing reaction tower, essence strain reaction tower, dehydration tower, dry reaction tower, finished product storage tower, effluent disposal system, acidification equipment, add alkali equipment, resin filtration system, naphthol recovery system, naphthol holding vessel, valve, flowmeter device are installed to the entrance of each pipeline, install thermometer, pressure gauge device in every tower. Can obtain naval stores, pitch and tar through this system. The utility model has the advantages of: the environmental protection and energy saving of process consideration looks, energy utilization is rateed highly, utilizes again after can purifying liquid waste, the sour product purity of 2 -3 through the preparation of this system is high, and more than 98.89%, the fusing point can reach 220 DEG C, and the percent crystallization in massecuite is less than 3%, and the finished product colour is the yellowish -brown, optimize the production technology, low in production cost, alkali lack raw material consumption, and the calorific value high -usage does not have tar and coking thing to generate, belongs to cleaner production technology.

Description

A kind of production system of industry preparation 2-carboxyl-3-naphthoic acid
Technical field
The utility model relates to a kind of production system of industry preparation 2-carboxyl-3-naphthoic acid, belongs to chemical field.
Background technology
2-3 acid (systematic naming method is 2-hydroxyl-3-naphthoic acid (2-Naphthoic-3-Hydroxylicacid)) is used as dyestuff (especially glacial dye), pigment dyestuff and medical important intermediate of producing, and it is that raw material forms through carboxylated with beta naphthal.223 acid producing waste waters derive from acid out, washing filtering workshop section, often produce 1t223 acid finished product, waste discharge 2 ~ 3m3.The organic content of waste water is high, acidity is large, saltiness is large, and biodegradability is very poor, and by methods such as general oxidation, coagulations, cost is high, is difficult to apply in Practical Project.Therefore, the object reaching improvement to this kind of waste water with the recovery realizing resource is crucial.On 2,3 of 2-3 acid naphthalene nucleus, there is hydroxyl and carboxyl respectively, dissociation can form organic anion, analyze theoretically, ionic association 2 preparing anion exchange extracting 2 system of stripping can be adopted to process.The technique of current synthesis is mainly divided into solid phase method and liquid phase method, although two kinds of each tool advantages of method, but the product ubiquity produced common problem: unstable product quality, be a bit darkish in color, particle is less, content is on the low side, have impact on its export competitiveness.Therefore, by the analysis to neutralization and acid out process, its output is improved.
Utility model content
For prior art Problems existing, the utility model uses a kind of production system of industry preparation 2-carboxyl-3-naphthoic acid, and this system comprises the first reaction tower, carboxylation reaction tower, the second reaction tower, neutralization reaction tower, acid precipitation reaction tower, press filtration reaction tower, essence filter reaction tower, dehydration reaction tower, dry reaction tower, finished product storage tower, Waste Water Treatment, acid adding equipment, adds alkali equipment, resin filter system, naphthols recovery system, naphthols hold-up vessel, wherein, the discharge port of naphthols hold-up vessel connects the feeding mouth of the first reaction tower by pipeline, the discharge port of the first reaction tower connects the feeding mouth of carboxylation reaction tower by pipeline, the discharge port of carboxylation reaction tower connects the feeding mouth of the second reaction tower by pipeline, the discharge port of the second reaction tower connects the feeding mouth of neutralization reaction tower by pipeline, the discharge port of neutralization reaction tower connects the feeding mouth of acid precipitation reaction tower by pipeline, the discharge port of acid precipitation reaction tower connects the feeding mouth of press filtration reaction tower by pipeline, the discharge port of press filtration reaction tower connects the feeding mouth of essence filter reaction tower by pipeline, the discharge port of essence filter reaction tower connects the feeding mouth of dehydration reaction tower by pipeline, the discharge port of dehydration reaction tower connects the feeding mouth of dry reaction tower by pipeline, the discharge port of dry reaction tower connects the feeding mouth of product storage tank by pipeline, the water port of press filtration reaction tower connects the first water inlet of Waste Water Treatment by pipeline, the water port of essence filter reaction tower connects the second water inlet of Waste Water Treatment by pipeline, the water port of dehydration reaction tower connects the 3rd water inlet of Waste Water Treatment by pipeline, the water port of dry reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline, what the first acid mouth of acid adding equipment connected the second reaction tower by pipeline enters sour mouth, what the second acid mouth of acid adding equipment connected neutralization reaction tower by pipeline enters sour mouth, what the 3rd acid mouth of acid adding equipment connected acid precipitation reaction tower by pipeline enters sour mouth, what the first alkali outlet adding alkali equipment connected the first reaction tower by pipeline enters alkali mouth, what the second alkali outlet adding alkali equipment connected neutralization reaction tower by pipeline enters alkali mouth, the resin outlet of the second reaction tower connects the feeding mouth of resin filtering system by pipeline, the discharge port of resin filter system connects the feeding mouth of naphthols recovery system by pipeline, the discharge port of naphthols recovery system connects the first feeding mouth of naphthols hold-up vessel by pipeline, the naphthols outlet of carboxylation reaction tower connects the second feeding mouth of naphthols hold-up vessel by pipeline, the process gas row mouth of Waste Water Treatment connects the air intake of carboxylation reaction tower by pipeline.
The ingress of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
Rosin products, pitch and tar can be obtained by this system.
Use the organic pollutant in industrial spirit extraction wastewater in Waste Water Treatment, final extract obtains water and carbonic acid gas by the mode of burning, and water extraction supplies the second reaction tower and uses, and carbonic acid gas is supplied to carboxylation reaction tower and uses.
Acid adding equipment use sulfuric acid, add alkali equipment use sodium hydroxide.
The utility model has the advantage of:
(1) processing condition phase environmental protection and energy saving, energy utilization rate is high, re-uses after can purifying liquid waste.
(2) the 2-3 acid product purity prepared by native system is high, and more than 98.89%, fusing point can reach 220 DEG C, and percent crystallization in massecuite is less than 3%, and finished color is yellowish brown.
(3) be optimized production technique, production cost is low, the few raw material consumption of alkali, and utilization rate of heat value is high, does not have tar and carbonizing matter to generate, belongs to process for cleanly preparing.
Accompanying drawing explanation
Fig. 1 is the production system schematic diagram of industry preparation 2-carboxyl-3-naphthoic acid.
1-first reaction tower, 2-carboxylation reaction tower, 3-second reaction tower, 4-neutralization reaction tower, 5-acid precipitation reaction tower, 6-press filtration reaction tower, 7-essence filter reaction tower, 8-dehydration reaction tower, 9-dry reaction tower, 10-finished product storage tower, 11-Waste Water Treatment, 12-acid adding equipment, 13-add alkali equipment, 14-resin filter system, 15-naphthols recovery system, 16-naphthols hold-up vessel.
Embodiment
The production system of a kind of industry preparation 2-carboxyl-3 naphthoic acid as shown in Figure 1, this system comprises the first reaction tower 1, carboxylation reaction tower 2, second reaction tower 3, neutralization reaction tower 4, acid precipitation reaction tower 5, press filtration reaction tower 6, essence filter reaction tower 7, dehydration reaction tower 8, dry reaction tower 9, finished product storage tower 10, Waste Water Treatment 11, acid adding equipment 12, adds alkali equipment 13, resin filter system 14, naphthols recovery system 15, naphthols hold-up vessel 16 etc.; Wherein, the discharge port of naphthols hold-up vessel 16 connects the feeding mouth of the first reaction tower 1 by pipeline, and the discharge port of the first reaction tower 1 connects the feeding mouth of carboxylation reaction tower 2 by pipeline, by calculating, throw in the beta naphthal of respective amount to the first reaction tower 1.Material is heated up, time in tower about material temperature rise to 110 DEG C, starts and stir, be rapidly heated to 125 DEG C ± 5 DEG C, be incubated 90 minutes.To be analyzed qualified after, feed liquid proceeds to carboxylation reaction tower 2; The discharge port of carboxylation reaction tower 2 connects the feeding mouth of the second reaction tower 3 by pipeline, be preheated to about 135 DEG C, starts stirring and carries out normal pressure dehydration.By in carboxylation reaction tower 2 because material is oxidized or coking and the resin object that generates is separated through diluted acid acidifying and water dilution postprecipitation.After temperature of charge rises to 170 DEG C and stablizes 30 minutes, close distillation valve boosting dehydration.When temperature rises to 235 DEG C, during pressure 0.2 ~ 0.3MPa, open condenser blow-off valve, distillation valve, sweep pipe with steam, pressure is dropped to normal pressure.Start water-ring pump to vacuumize simultaneously, carry out negative-pressure operation.When vacuum tightness reaches-0.08MPa, start vapor jet pump, stop water-ring pump, and continue negative-pressure operation.Treat that temperature of charge rises to 235 DEG C, steam temperature about 170 DEG C, close distillation valve, vacuum valve, open condenser exhaust-valve, vapor jet pump of stopping using, stop stirring, pressure liter is caused normal pressure.Then pass into CO 2gas, carries out examination carboxylation reaction, CO 2pressure is about 0.4 ~ 0.6MPa.When the CO2 in still absorbs comparatively slowly, stop passing into CO 2, start to stir and continue reaction.When temperature rises to about 250 DEG C, start water-ring pump simultaneously, carry out beta naphthal distillation procedure, when temperature of charge is down to 225 DEG C ± 5 DEG C, steam temperature 170 DEG C, stops distillation, and stop using water-ring pump and squirt pump stop stirring.Again pass into CO to carboxylation pot 2gas, when carboxylation reaction is slow, stops for CO 2, start stirring again, then continue to pass into CO 2, CO 2pressure 0.4 ~ 0.6MPa.When temperature of charge rises to 265 DEG C, start water-ring pump, distillation procedure is carried out to material.Treat that vacuum tightness rises to-0.08MPa, and when stablizing, water-ring pump of stopping using, only continues distillation with squirt pump.When vacuum tightness rises to-0.094MPa, and during without flow, this distillation is complete, then repeats above-mentioned steps operation, until when overhead product shows red, carboxylation reaction completes substantially.When pressure is normal pressure, put into boiling water, start and stir, discharging after about 15 minutes, proceeds to the second reaction tower 3.The discharge port of the second reaction tower 3 connects the feeding mouth of neutralization reaction tower 4 by pipeline, when temperature rise to 80 DEG C, close open steam valve, and connect the next material of pressure and bitumen recovery water, waste water desorption height dope etc., start and stir, adjustment temperature of charge to 55 ~ 60 DEG C, slowly added diluted acid after 40 minutes, material pH value is adjusted to 6.5 ~ 7.0, continues to stir half an hour.Stop stirring, leave standstill 40 minutes, add water.Stir lower intensification and be heated to boiling, then stop to stir standing 40 minutes, discharge pitch, when discharge show look, stop discharge.The discharge port of neutralization reaction tower 4 connects the feeding mouth of acid precipitation reaction tower 5 by pipeline, during when the temperature to 55 ~ 60 DEG C, steam off, after pH detection is qualified, opens coiled pipe cooling inlet/outlet valve, cool.When temperature of charge is down to 40 ~ 45 DEG C, closes water coolant, evenly add solid sodium bicarbonate, when pH value is adjusted to 6 ~ 6.3, stirs after 30 minutes, again detect pH value; After pH value is qualified, continue to use industrial water for cooling.When temperature is down to 35 DEG C, stop using service water, then continue cooling with freezing clear water.Cooling is stopped when temperature is down to 20 DEG C.The discharge port of acid precipitation reaction tower 5 connects the feeding mouth of press filtration reaction tower 6 by pipeline, 78 ~ 80 DEG C are warming up to steam, to acid precipitation reaction tower 5 acid adding, when pH value is 1 ~ 2, suspends acid adding, stir after 20 minutes, after analysis is qualified, open coiled pipe water coolant turnover valve, be cooled to 55 ~ 60 DEG C, stop stirring.Leave standstill after 30 minutes, supernatant liquid is discharged.The discharge port of press filtration reaction tower 6 connects the feeding mouth of essence filter reaction tower 7 by pipeline, when whizzer charging reaches 80%, stop charging, use filtered water washing leaching cake.Filter cake picks up, and sends into filter cake yard, use to be dried.The discharge port of essence filter reaction tower 7 connects the feeding mouth of dehydration reaction tower 8 by pipeline, the discharge port of dehydration reaction tower 8 connects the feeding mouth of dry reaction tower 9 by pipeline, the discharge port of dry reaction tower 9 connects the feeding mouth of product storage tank 10 by pipeline, the water port of press filtration reaction tower 6 connects the first water inlet of Waste Water Treatment 11 by pipeline, the water port of essence filter reaction tower 7 connects the second water inlet of Waste Water Treatment 11 by pipeline, the water port of dehydration reaction tower 8 connects the 3rd water inlet of Waste Water Treatment 11 by pipeline, the water port of dry reaction tower 9 connects the 4th water inlet of Waste Water Treatment 11 by pipeline, what the first acid mouth of acid adding equipment 12 connected the second reaction tower 3 by pipeline enters sour mouth, what the second acid mouth of acid adding equipment 12 connected neutralization reaction tower 4 by pipeline enters sour mouth, what the 3rd acid mouth of acid adding equipment 12 connected acid precipitation reaction tower 5 by pipeline enters sour mouth, what the first alkali outlet adding alkali equipment 13 connected the first reaction tower 1 by pipeline enters alkali mouth, what the second alkali outlet adding alkali equipment 13 connected neutralization reaction tower 4 by pipeline enters alkali mouth, the resin outlet of the second reaction tower 2 connects the feeding mouth of resin filtering system 14 by pipeline, the discharge port of resin filter system 14 connects the feeding mouth of naphthols recovery system 15 by pipeline, the discharge port of naphthols recovery system 15 connects the first feeding mouth of naphthols hold-up vessel 16 by pipeline, the naphthols outlet of carboxylation reaction tower 2 connects the second feeding mouth of naphthols hold-up vessel 16 by pipeline, the process gas row mouth of Sewage treatment systems 11 connects the air intake of carboxylation reaction tower 2 by pipeline.
The production technique of industry preparation 2-carboxyl-3 naphthoic acid, the ingress of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
The production technique of industry preparation 2-carboxyl-3 naphthoic acid, can obtain rosin products, pitch and tar by this system.
The production technique of industry preparation 2-carboxyl-3 naphthoic acid, the organic pollutant in industrial spirit extraction wastewater is used in Waste Water Treatment, final extract obtains water and carbonic acid gas by the mode of burning, and water extraction supplies the second reaction tower and uses, and carbonic acid gas is supplied to carboxylation reaction tower and uses.
The production technique of industry preparation 2-carboxyl-3 naphthoic acid, acid adding equipment use sulfuric acid, adds alkali equipment use sodium hydroxide.

Claims (2)

1. the production system of an industry preparation 2-carboxyl-3-naphthoic acid, it is characterized in that, this system comprises the first reaction tower, carboxylation reaction tower, the second reaction tower, neutralization reaction tower, acid precipitation reaction tower, press filtration reaction tower, essence filter reaction tower, dehydration reaction tower, dry reaction tower, finished product storage tower, Waste Water Treatment, acid adding equipment, adds alkali equipment, resin filter system, naphthols recovery system, naphthols hold-up vessel, wherein, the discharge port of naphthols hold-up vessel connects the feeding mouth of the first reaction tower by pipeline, the discharge port of the first reaction tower connects the feeding mouth of carboxylation reaction tower by pipeline, the discharge port of carboxylation reaction tower connects the feeding mouth of the second reaction tower by pipeline, the discharge port of the second reaction tower connects the feeding mouth of neutralization reaction tower by pipeline, the discharge port of neutralization reaction tower connects the feeding mouth of acid precipitation reaction tower by pipeline, the discharge port of acid precipitation reaction tower connects the feeding mouth of press filtration reaction tower by pipeline, the discharge port of press filtration reaction tower connects the feeding mouth of essence filter reaction tower by pipeline, the discharge port of essence filter reaction tower connects the feeding mouth of dehydration reaction tower by pipeline, the discharge port of dehydration reaction tower connects the feeding mouth of dry reaction tower by pipeline, the discharge port of dry reaction tower connects the feeding mouth of product storage tank by pipeline, the water port of press filtration reaction tower connects the first water inlet of Waste Water Treatment by pipeline, the water port of essence filter reaction tower connects the second water inlet of Waste Water Treatment by pipeline, the water port of dehydration reaction tower connects the 3rd water inlet of Waste Water Treatment by pipeline, the water port of dry reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline, what the first acid mouth of acid adding equipment connected the second reaction tower by pipeline enters sour mouth, what the second acid mouth of acid adding equipment connected neutralization reaction tower by pipeline enters sour mouth, what the 3rd acid mouth of acid adding equipment connected acid precipitation reaction tower by pipeline enters sour mouth, what the first alkali outlet adding alkali equipment connected the first reaction tower by pipeline enters alkali mouth, what the second alkali outlet adding alkali equipment connected neutralization reaction tower by pipeline enters alkali mouth, the resin outlet of the second reaction tower connects the feeding mouth of resin filtering system by pipeline, the discharge port of resin filter system connects the feeding mouth of naphthols recovery system by pipeline, the discharge port of naphthols recovery system connects the first feeding mouth of naphthols hold-up vessel by pipeline, the naphthols outlet of carboxylation reaction tower connects the second feeding mouth of naphthols hold-up vessel by pipeline, the venting port of Waste Water Treatment connects the air intake of carboxylation reaction tower by pipeline.
2. production system according to claim 1, is characterized in that, the ingress of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
CN201520390917.7U 2015-06-09 2015-06-09 Production system of industry preparation 2 - carboxyl - 3 - naphthoic acid Withdrawn - After Issue CN204752566U (en)

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CN201520390917.7U CN204752566U (en) 2015-06-09 2015-06-09 Production system of industry preparation 2 - carboxyl - 3 - naphthoic acid

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CN201520390917.7U CN204752566U (en) 2015-06-09 2015-06-09 Production system of industry preparation 2 - carboxyl - 3 - naphthoic acid

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Granted publication date: 20151111

Effective date of abandoning: 20161019

C25 Abandonment of patent right or utility model to avoid double patenting