CN104860816B - Production system for industrially preparing 2-hydroxyl-3-naphthoic acid - Google Patents

Production system for industrially preparing 2-hydroxyl-3-naphthoic acid Download PDF

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CN104860816B
CN104860816B CN201510310422.3A CN201510310422A CN104860816B CN 104860816 B CN104860816 B CN 104860816B CN 201510310422 A CN201510310422 A CN 201510310422A CN 104860816 B CN104860816 B CN 104860816B
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reaction tower
pipeline
connects
acid
feeding mouth
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CN104860816A (en
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李宇钟
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Suqian Siruiyi New Materials Co ltd
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Jinhua Zhichan Wuyuan Information Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/15Preparation of carboxylic acids or their salts, halides or anhydrides by reaction of organic compounds with carbon dioxide, e.g. Kolbe-Schmitt synthesis

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a production system for industrially preparing 2-carboxyl-3-naphthoic acid, which comprises a first reaction tower, a carboxylation reaction tower, a second reaction tower, a neutralization reaction tower, an acidification reaction tower, a filter pressing reaction tower, a fined filtration reaction tower, a dehydration reaction tower, a drying reaction tower, a finished product storage tower, a wastewater treatment system, an acid adding device, an alkali adding device, a resin filter system, a naphthol recovering system and a naphthol storage tank. Industrial alcohol is used in the wastewater treatment system to extract organic pollutants in wastewater, then extractant is combusted to obtain water and carbon dioxide, the obtained water is supplied to the second reaction tower for use, and the obtained carbon dioxide is supplied to the carboxylation reaction tower for use. The product is high in purity up to more than 98.89%, is high in melting point up to 220 DEG C, the crystallization rate is less than 3%, and the finished product is yellowish-brown.

Description

A kind of industrially prepared 2- Hydroxyl -3- The production system of naphthoic acid
Technical field
The present invention relates to a kind of production system of industrially prepared 2- hydroxyl -3 naphthoic acid, belong to chemical field.
Background technology
2-3 acid (systematic naming method is 2- hydroxyl -3- naphthoic acid (2-Naphthoic-3-Hydroxylicacid)) is used as the important intermediate that dyestuff (especially azoic dyes), organic pigment and medicine produce, and it is formed through carboxylated with beta naphthal for raw material.223 acid producing waste waters derive from acid out, washing filtering workshop section, often produce 1t223 acid finished product, waste discharge 2~3m3.The content of organics of waste water is high, acidity is big, salinity is big, and biodegradability is very poor, and with methods such as general oxidation, coagulations, high cost is it is difficult to apply in Practical Project.Therefore, the purpose reaching improvement to this kind of waste water with the recovery realizing resource is crucial.On 2,3 of 2-3 acid naphthalene nucleus, it is respectively provided with hydroxyl and carboxyl, formation organic anion can be dissociated, theoretically analyze, can be processed using ion association 2 preparing anion exchange extracting 2 back extraction system.At present the technique of synthesis is broadly divided into solid phase method and liquid phase method, although two methods respectively have an advantage, the product generally existing produced common problem:Unstable product quality, be a bit darkish in color, granule is less, content is low, have impact on its export competitiveness.Therefore, by the analysis to neutralization and acid out process, improve its yield.
Content of the invention
The problem existing for prior art, the present invention uses a kind of production system of industrially prepared 2- hydroxyl -3- naphthoic acid, and this system includes the first reaction tower, carboxylation reaction tower, the second reaction tower, neutralization reaction tower, acid precipitation reaction tower, filter pressing reaction tower, fine straining reaction tower, dehydration tower, dry reaction tower, finished product storage tower, Waste Water Treatment, acid adding equipment, adds alkali equipment, resin filter system, naphthols recovery system, naphthols holding vessel;Wherein,The discharging opening of naphthols holding vessel connects the feeding mouth of the first reaction tower by pipeline,The discharging opening of the first reaction tower connects the feeding mouth of carboxylation reaction tower by pipeline,The discharging opening of carboxylation reaction tower connects the feeding mouth of the second reaction tower by pipeline,The discharging opening of the second reaction tower connects the feeding mouth of neutralization reaction tower by pipeline,The discharging opening of neutralization reaction tower connects the feeding mouth of acid precipitation reaction tower by pipeline,The discharging opening of acid precipitation reaction tower connects the feeding mouth of filter pressing reaction tower by pipeline,The discharging opening of filter pressing reaction tower connects the feeding mouth of fine straining reaction tower by pipeline,The discharging opening of fine straining reaction tower connects the feeding mouth of dehydration tower by pipeline,The discharging opening of dehydration tower connects the feeding mouth of dry reaction tower by pipeline,The discharging opening of dry reaction tower connects the feeding mouth of product storage tank by pipeline,The discharge outlet of filter pressing reaction tower connects the first water inlet of Waste Water Treatment by pipeline,The discharge outlet of fine straining reaction tower connects the second water inlet of Waste Water Treatment by pipeline,The discharge outlet of dehydration tower connects the 3rd water inlet of Waste Water Treatment by pipeline,The discharge outlet of dry reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline,First acid mouth of acid adding equipment enters sour mouth by pipeline connection the second reaction tower,Second acid mouth of acid adding equipment enters sour mouth by pipeline connection neutralization reaction tower,3rd acid mouth of acid adding equipment enters sour mouth by pipeline connection acid precipitation reaction tower,Plus the first alkali outlet of alkali equipment by pipeline connect the first reaction tower enter alkali mouth,Plus the second alkali outlet of alkali equipment by pipeline connect neutralization reaction tower enter alkali mouth,The resin outlet of the second reaction tower connects the feeding mouth of resin filtration system by pipeline,The discharging opening of resin filter system connects the feeding mouth of naphthols recovery system by pipeline,The discharging opening of naphthols recovery system connects the first feeding mouth of naphthols holding vessel by pipeline,The naphthols outlet of carboxylation reaction tower connects the second feeding mouth of naphthols holding vessel by pipeline,The air intake that mouth connects carboxylation reaction tower by pipeline is arranged in place's qi-regulating of Waste Water Treatment.
The porch of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
Naval stores, Colophonium and tar can be obtained by this system.
Using the organic pollution in industrial alcohol extraction wastewater in Waste Water Treatment, final extract obtains water and carbon dioxide by way of burning, and water extraction supply the second reaction tower uses, and carbon dioxide is supplied to carboxylation reaction tower and uses.
Acid adding equipment using sulphuric acid, plus alkali equipment use sodium hydroxide.
It is an advantage of the current invention that:
(1)Process conditions phase environmental protection and energy saving, energy utilization rate is high, re-uses after can purifying waste water.
(2)The 2-3 acid product purity prepared by the system is high, and more than 98.89%, up to 220 DEG C, percent crystallization in massecuite is less than 3% to fusing point, and finished color is in yellowish-brown.
(3)Production technology is optimized, low production cost, the few consumption of raw materials of alkali, utilization rate of heat value is high, does not have tar and carbonizing matter to generate, belong to process for cleanly preparing.
Brief description
Fig. 1 is the production technology schematic diagram of industrially prepared 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- filter pressing reaction tower, 7- fine straining reaction tower, 8- dehydration 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 holding vessel.
Specific embodiment
The production system of a kind of industrially prepared 2- hydroxyl -3 naphthoic acid as shown in Figure 1, this system includes the first reaction tower 1, carboxylation reaction tower 2, the second reaction tower 3, neutralization reaction tower 4, acid precipitation reaction tower 5, filter pressing reaction tower 6, fine straining reaction tower 7, dehydration 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 holding vessel 16 etc.;Wherein, the discharging opening of naphthols holding vessel 16 connects the feeding mouth of the first reaction tower 1 by pipeline, and the discharging opening of the first reaction tower 1 connects the feeding mouth of carboxylation reaction tower 2 by pipeline, by calculating, throws in the beta naphthal of respective amount to the first reaction tower 1.Material is heated up, when material temperature rise is to 110 DEG C about in tower, starts stirring, 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 discharging opening of carboxylation reaction tower 2 connects the feeding mouth of the second reaction tower 3 by pipeline, is preheated to 135 DEG C about, 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 dilutes postprecipitation through diluted acid acidifying and water and separates.After temperature of charge rises to 170 DEG C and stablizes 30 minutes, close distillation valve and rise press-dehydrating.When temperature rises to 235 DEG C, during pressure 0.2~0.3MPa, open condenser atmospheric valve, distillation valve, sweep pipe with steam, pressure is dropped to normal pressure.Start water ring pump evacuation simultaneously, carry out negative-pressure operation.When vacuum reaches -0.08MPa, start steam jet pump, stop water ring pump, and continue negative-pressure operation.Treat that temperature of charge rises to 235 DEG C, 170 DEG C about of steam temperature, close distillation valve, vacuum valve, open condenser exhaust-valve, disable steam jet pump, stop stirring, pressure is risen and causes normal pressure.Then it is passed through CO2Gas, carries out trying carboxylation reaction, CO2Pressure is about 0.4~0.6MPa.As the CO in kettle2When absorbing more slow, stop being passed through CO2, start stirring and continue reaction.When temperature rises to 250 DEG C about, start water ring pump simultaneously, carry out beta naphthal distillation procedure, when temperature of charge is down to 225 DEG C ± 5 DEG C, 170 DEG C of steam temperature, stop distillation, disable water ring pump and ejector pump, stop stirring.It is passed through CO to carboxylation pot again2Gas, when carboxylation reaction is slow, stops supplying CO2, start stirring again, then proceed to be passed through CO2, CO2Pressure 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 rises to -0.08MPa, and when stablizing, disable water ring pump, only continue distillation with ejector pump.When vacuum rises to -0.094MPa, and no flow when, this distillation finishes, and repeats above-mentioned steps operation, until when distillation shows red, carboxylation reaction is basically completed.When pressure is for normal pressure, put into boiling water, start stirring, discharging after about 15 minutes, proceed to the second reaction tower 3.The discharging opening of the second reaction tower 3 connects the feeding mouth of neutralization reaction tower 4 by pipeline, when temperature rise is to 80 DEG C, close live (open) steam valve, and connect material and bitumen recovery water, waste water high dope of desorption etc. that pressure is come, start stirring, adjustment temperature of charge, to 55~60 DEG C, slowly adds diluted acid after 40 minutes, material pH value is adjusted to 6.5~7.0, continues stirring half an hour.Stop stirring, stand 40 minutes, add water.The lower intensification of stirring is heated to seething with excitement, and then stops stirring standing 40 minutes, discharges Colophonium, when emission show color, stops discharge.The discharging opening 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, and after pH detection is qualified, opens coiled pipe cooling inlet/outlet valve, cooled down.When temperature of charge is down to 40~45 DEG C, closes cooling water, be uniformly added into solid sodium bicarbonate, when pH value adjusts to 6~6.3, after stirring 30 minutes, detect pH value again;After pH value is qualified, continuation industry water is lowered the temperature.When temperature is down to 35 DEG C, stop using industry water, then continue cooling with freezing clear water.Stop cooling when temperature is down to 20 DEG C.The discharging opening of acid precipitation reaction tower 5 connects the feeding mouth of filter pressing reaction tower 6 by pipeline, it is warming up to 78~80 DEG C with steam, to acid precipitation reaction tower 5 acid adding, when pH value is 1~2, suspend acid adding, after stirring 20 minutes, after analyzing qualified, open coiled pipe cooling water turnover valve, be cooled to 55~60 DEG C, stop stirring.Standing, after 30 minutes, the supernatant is discharged.The discharging opening of filter pressing reaction tower 6 connects the feeding mouth of fine straining reaction tower 7 by pipeline, when centrifuge charging reaches 80%, stops charging, washs filter cake with filter water.Filter cake picks up, and sends into filter cake yard, use to be dried.The discharging opening of fine straining reaction tower 7 connects the feeding mouth of dehydration tower 8 by pipeline,The discharging opening of dehydration tower 8 connects the feeding mouth of dry reaction tower 9 by pipeline,The discharging opening of dry reaction tower 9 connects the feeding mouth of product storage tank 10 by pipeline,The discharge outlet of filter pressing reaction tower 6 connects the first water inlet of Waste Water Treatment 11 by pipeline,The discharge outlet of fine straining reaction tower 7 connects the second water inlet of Waste Water Treatment 11 by pipeline,The discharge outlet of dehydration tower 8 connects the 3rd water inlet of Waste Water Treatment 11 by pipeline,The discharge outlet of dry reaction tower 9 connects the 4th water inlet of Waste Water Treatment 11 by pipeline,First acid mouth of acid adding equipment 12 enters sour mouth by pipeline connection the second reaction tower 3,Second acid mouth of acid adding equipment 12 enters sour mouth by pipeline connection neutralization reaction tower 4,3rd acid mouth of acid adding equipment 12 enters sour mouth by pipeline connection acid precipitation reaction tower 5,Plus the first alkali outlet of alkali equipment 13 by pipeline connect the first reaction tower 1 enter alkali mouth,Plus the second alkali outlet of alkali equipment 13 by pipeline connect neutralization reaction tower 4 enter alkali mouth,The resin outlet of the second reaction tower 2 connects the feeding mouth of resin filtration system 14 by pipeline,The discharging opening of resin filter system 14 connects the feeding mouth of naphthols recovery system 15 by pipeline,The discharging opening of naphthols recovery system 15 connects the first feeding mouth of naphthols holding vessel 16 by pipeline,The naphthols outlet of carboxylation reaction tower 2 connects the second feeding mouth of naphthols holding vessel 16 by pipeline,The air intake that mouth connects carboxylation reaction tower 2 by pipeline is arranged in place's qi-regulating of sewage disposal system 11.
The production technology of industrially prepared 2- hydroxyl -3 naphthoic acid, the porch of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
The production technology of industrially prepared 2- hydroxyl -3 naphthoic acid, can obtain naval stores, Colophonium and tar by this system.
The production technology of industrially prepared 2- hydroxyl -3 naphthoic acid, using the organic pollution in industrial alcohol extraction wastewater in Waste Water Treatment, final extract obtains water and carbon dioxide by way of burning, and water extraction supply the second reaction tower uses, and carbon dioxide is supplied to carboxylation reaction tower and uses.
The production technology of industrially prepared 2- hydroxyl -3 naphthoic acid, acid adding equipment using sulphuric acid, plus alkali equipment use sodium hydroxide.

Claims (4)

1. a kind of production system of industrially prepared 2- hydroxyl -3- naphthoic acid, it is characterized in that, this system includes the first reaction tower, carboxylation reaction tower, the second reaction tower, neutralization reaction tower, acid precipitation reaction tower, filter pressing reaction tower, fine straining reaction tower, dehydration tower, dry reaction tower, finished product storage tower, Waste Water Treatment, acid adding equipment, adds alkali equipment, resin filter system, naphthols recovery system, naphthols holding vessel;Wherein,The discharging opening of naphthols holding vessel connects the feeding mouth of the first reaction tower by pipeline,The discharging opening of the first reaction tower connects the feeding mouth of carboxylation reaction tower by pipeline,The discharging opening of carboxylation reaction tower connects the feeding mouth of the second reaction tower by pipeline,The discharging opening of the second reaction tower connects the feeding mouth of neutralization reaction tower by pipeline,The discharging opening of neutralization reaction tower connects the feeding mouth of acid precipitation reaction tower by pipeline,The discharging opening of acid precipitation reaction tower connects the feeding mouth of filter pressing reaction tower by pipeline,The discharging opening of filter pressing reaction tower connects the feeding mouth of fine straining reaction tower by pipeline,The discharging opening of fine straining reaction tower connects the feeding mouth of dehydration tower by pipeline,The discharging opening of dehydration tower connects the feeding mouth of dry reaction tower by pipeline,The discharging opening of dry reaction tower connects the feeding mouth of product storage tank by pipeline,The discharge outlet of filter pressing reaction tower connects the first water inlet of Waste Water Treatment by pipeline,The discharge outlet of fine straining reaction tower connects the second water inlet of Waste Water Treatment by pipeline,The discharge outlet of dehydration tower connects the 3rd water inlet of Waste Water Treatment by pipeline,The discharge outlet of dry reaction tower connects the 4th water inlet of Waste Water Treatment by pipeline,First acid mouth of acid adding equipment enters sour mouth by pipeline connection the second reaction tower,Second acid mouth of acid adding equipment enters sour mouth by pipeline connection neutralization reaction tower,3rd acid mouth of acid adding equipment enters sour mouth by pipeline connection acid precipitation reaction tower,Plus the first alkali outlet of alkali equipment by pipeline connect the first reaction tower enter alkali mouth,Plus the second alkali outlet of alkali equipment by pipeline connect neutralization reaction tower enter alkali mouth,The resin outlet of the second reaction tower connects the feeding mouth of resin filtration system by pipeline,The discharging opening of resin filter system connects the feeding mouth of naphthols recovery system by pipeline,The discharging opening of naphthols recovery system connects the first feeding mouth of naphthols holding vessel by pipeline,The naphthols outlet of carboxylation reaction tower connects the second feeding mouth of naphthols holding vessel by pipeline,The air vent of Waste Water Treatment connects the air intake of carboxylation reaction tower by pipeline.
2. the production system of industrially prepared 2- hydroxyl -3- naphthoic acid according to claim 1, it is characterised in that the porch of each pipeline is provided with valve, flowermeter, is provided with thermometer, pressure gage device in each tower.
3. the production system of industrially prepared 2- hydroxyl -3- naphthoic acid according to claim 1, it is characterized in that, using the organic pollution in industrial alcohol extraction wastewater in Waste Water Treatment, final extract obtains water and carbon dioxide by way of burning, water extraction supply the second reaction tower uses, and carbon dioxide is supplied to carboxylation reaction tower and uses.
4. industrially prepared 2- hydroxyl -3- naphthoic acid according to claim 1 production system it is characterised in that acid adding equipment using sulphuric acid, plus alkali equipment use sodium hydroxide.
CN201510310422.3A 2015-06-09 2015-06-09 Production system for industrially preparing 2-hydroxyl-3-naphthoic acid Active CN104860816B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4239913A (en) * 1977-10-25 1980-12-16 Kabushiki Kaisha Veno Seiyaku Oyo Kenkyujo Process for preparing 2-hydroxynaphthalenecarboxylic acids
ES8107146A1 (en) * 1979-12-25 1981-10-16 Sumitomo Chemical Co Process for producing 2 hydroxy-naphthalene-3-carboxylic acid
JPS61115053A (en) * 1984-11-09 1986-06-02 Ueno Seiyaku Oyo Kenkyusho:Kk Production of aromatic hydroxycarboxylic acid
DE4316933A1 (en) * 1993-05-21 1994-11-24 Hoechst Ag Process for the preparation of aromatic hydroxycarboxylic acids
CN102816063B (en) * 2012-09-10 2014-06-11 济宁阳光煤化有限公司 Method for producing high purity 2-hydroxy-3-naphthoic acid
CN104447302A (en) * 2014-12-29 2015-03-25 唐山市丰南区佳跃化工产品有限公司 Method of improving content of 2-hydroxy-3-naphthoic acid produced in gas-solid phase method
CN104649898B (en) * 2015-02-16 2016-09-28 曲靖众一合成化工有限公司 A kind of solvent method continuous carbonization produces beta naphthal, the method and device of coproduction 2,3 acid

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