CN103214388B - A kind of recoverying and utilizing method of nitrating wasting acid - Google Patents
A kind of recoverying and utilizing method of nitrating wasting acid Download PDFInfo
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- CN103214388B CN103214388B CN201210018863.2A CN201210018863A CN103214388B CN 103214388 B CN103214388 B CN 103214388B CN 201210018863 A CN201210018863 A CN 201210018863A CN 103214388 B CN103214388 B CN 103214388B
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Abstract
The invention provides a kind of recoverying and utilizing method of nitrating wasting acid, the nitrating wasting acid mother liquor that the method produces with p acetamidoanisol and mixed acid nitrification is for raw material, by neutralization, cold filtration, separating organic matters, decolouring oxidation, condensing crystal producing ammonium sulfate byproduct, the organic itrated compound be separated then returns as nitrated raw material, improve the yield of nitration product, concentrated condensing hot air furnace is used for the washing of nitrated filter cake, solve the dirty slag disposal difficulties of calcium sulfate that nitrating wasting acid adopts limestone vegetation to produce because of low cannot the concentrating of sulfuric acid content usually, and by being separated, organic nitrated material in waste acid recovery returns as nitrated raw material, improve the yield of nitration product, thus really achieve the comprehensive utilization of waste acid resource.
Description
(1) technical field
The present invention relates to the recoverying and utilizing method of nitrating wasting acid in a kind of Chemical Manufacture, particularly the recoverying and utilizing method of nitrating wasting acid in amino-4 acetamido methyl-phenoxide production processes of a kind of 2-.
(2) background technology
Amino 4-acetamido methyl-phenoxide (being commonly called as reduzate) of 2-is the important intermediate of synthesis azoic dyestuff and medicine, is mainly used in the production of blueness, black azo dispersion dyes.Domestic production 2-amino-4-acetyl-anisidine is normally raw material with Para-Anisidine, through acidylate, nitrated, the processes such as reduction obtain, wherein, in nitrifying process, p acetamidoanisol and nitration mixture react and generate 2-nitro-4-acetyl-anisidine, add large water gaging again to carry out diluting and washing, to be separated better and to obtain nitration product, but also produce a large amount of nitrating wasting acids simultaneously, in this spent acid, sulfuric acid content is about 25%-30%, and be dissolved with part nitration product and other by-product impurities, organic content is at 0.2%-0.5%, COD is up to 5000mg/L, because of spent acid acidity, organic content is higher, if directly discharge, by serious pollution of ecological environment.
In view of nitrating wasting acid is a kind of severe corrosive and reluctant industrial waste, also part nitration product and unreacted raw material is dissolved with in spent acid, also be a kind of potential Sulphur ressource simultaneously, the increasingly stringent of and environmental requirement in short supply along with domestic Sulphur ressource, carrying out recycling to nitrating wasting acid, is the inevitable choice realizing Sustainable development.Industrial, spent acid process adopts the methods such as Waste Sulfuric Acid is concentrated, Pintsch process, production phosphate fertilizer, extraction, neutralizing treatment, although the improvement of the dilute sulphuric acid that the mixed acid nitrification of arene produces has ubiquity very much in fine chemistry industry is produced, but the difference of nitrification process, the improvement of nitrating wasting acid also has difference technically, and above-mentioned each method has certain applicable elements and respective limitation.
Such as, adopt concentration technology process spent acid, no matter be that traditional with serious pollution cooking-pot type concentrates or vacuum concentration, generally all require sulfuric acid concentration higher (more than 60%) in spent acid, it is high without economic worth that low-concentration waste acid concentrates energy consumption, and during vacuum concentration, the high-enriched organics impurity in spent acid is unfavorable for that subsequent sulphuric acid concentrates and recycling, and sulphuric acid concentration requires high to equipment material, facility investment is larger; And Pintsch process mode is applicable to that sulfuric acid concentration in spent acid is higher, containing the situation of a large amount of combustiblecomponents, but its scale of investment is large, process energy consumption is higher, is unsuitable for the process of nitrating wasting acid.The nitrating wasting acid of employing is in the past applied to production of phosphate fertilizer, is also limited because the toxic substance in spent acid can cause serious harm to farm crop.
In addition, patent " a kind of production technique of preparing nitrogenous fertilizer by recycling industry nitration waste mixed " (CN200710018694) provides a kind of production technique of preparing nitrogenous fertilizer by recycling industry nitration waste mixed.Utilize the nitrating wasting acid of sulfur acid 65 ~ 80% and ammonium bicarbonate soln to react, reaction feed liquid produces nitrogenous fertilizer by flash concentration.But this patent mainly for be the spent acid that sulfuric acid concentration is higher, the process of the organic impurities in nitrating wasting acid is not addressed, and sulfuric acid concentration contained by nitrating wasting acid is lower in reduzate production, containing large amount of organic in spent acid, the nitration product of contain in spent acid about 0.5% and raw material, after Separation and Recovery, return and can improve nitration product yield as nitrated raw material.
The spent acid that in producing for reduzate, nitrated operation produces, adopts above-mentioned each method process all undesirable.Domestic not yet have efficient reduzate nitrating wasting acid recycling and treatment technology, and limited control measures is adopt carbide slag neutralizing treatment at the most, produces a large amount of containing organic calcium sulfate solid waste.
The nitrated operation production process of reduzate needs massive laundering to wash, the organism of nitrated separation, if spent acid neutralizing treatment, organism are reclaimed, water resources reclaims and produces chemical fertilizer and combine, effectively can solve reduzate and produce the process problem of nitrating wasting acid and realize the comprehensive utilization of resources of nitrifying process.
(3) summary of the invention
The present invention aims to provide a kind of recoverying and utilizing method of nitrating wasting acid, the nitrating wasting acid mother liquor that the method produces with p acetamidoanisol and mixed acid nitrification is for raw material, by neutralization, cold filtration, separating organic matters, decolouring oxidation, condensing crystal producing ammonium sulfate byproduct, the organic itrated compound be separated then returns as nitrated raw material, improve the yield of nitration product, concentrated condensing hot air furnace is used for the washing of nitrated filter cake, thus realizes circulation, the comprehensive utilization of waste acid resource.
The technical solution used in the present invention is as follows:
A recoverying and utilizing method for nitrating wasting acid, described method comprises:
(1) spent acid neutralization: (wherein sulfuric acid content is about 25 ~ 30% for collection p acetamidoanisol and nitration mixture (sulfuric acid+nitric acid) reacted nitrating wasting acid mother liquor, w/w), pass into ammonia under stirring or add liquefied ammonia that to be neutralized to pH value be 5 ~ 7, obtain neutralizer;
(2) separating organic matters: the neutralizer of step (1) is cooled to 20 ~ 40 DEG C, separate out solid (itrated compound of dissolving and unreacted raw material) through press filtration or centrifugation, return as nitrated operation raw material after recovery, residue neutralizer carries out next step operation;
(3) purification and impurity removal: step (2) residue neutralizer carries out purification and impurity removal with activated carbon decolorizing or activated carbon decolorizing with the oxidizing mode of combining, described activated carbon decolorizing is for adding gac insulated and stirred 0.25 ~ 2 hour at 20 DEG C ~ 50 DEG C, described oxidizing for adding oxygenant insulated and stirred 0.25 ~ 2 hour at 20 ~ 35 DEG C; When the mode adopting decolorizing with activated carbon and oxygenant to combine purifies neutralizer, the mode reoxidized of first decolouring can be taked, also can take the mode of initial oxidation rear decoloring.
(4) condensing crystal: the neutralizer in step (3) after purification and impurity removal, through concentrated, crystallization, obtains solid ammonium sulfate, recycling condensing water.Concentrated can adopt that conventional single-action is concentrated, Multi-effect concentration, the mode of vapor recompression concentrated (MVR concentrates) also can be taked to carry out, and concentrated water of condensation can all reclaim as nitration product washing water, realizes the recycle of water resources.Crystalline mother solution then returns concentration systems, also partly can return purification system, removes the impurity of enrichment further, ensures the stay in grade of ammonium sulfate.The ammonium sulfate of purifying directly as product, also dryly further can obtain the lower product of water content.
Oxygenant is one of following or wherein two or more mixture in described step (3): clorox, hydrogen peroxide, dioxide peroxide, ozone, and its quality consumption is 0.02% ~ 1% of the described neutralizer quality of step (3); Described quality of activated carbon consumption be step (3) described in and liquid measure 0.05% ~ 2%.
Beneficial effect of the present invention is mainly reflected in: present invention achieves the process of nitrating wasting acid and the comprehensive utilization of resource in reduzate production, nitrating wasting acid neutralizes through ammonia, separation of organic substances, purification and impurity removal, producing ammonium sulfate byproduct product after the measures such as condensing crystal, recycling condensing water is in the filter cake washing of nitration product, solve the dirty slag disposal difficulties of calcium sulfate that nitrating wasting acid adopts limestone vegetation to produce because of low cannot the concentrating of sulfuric acid content usually, and by being separated, organic nitrated material in waste acid recovery returns as nitrated raw material, improve the yield of nitration product, thus really achieve the comprehensive utilization of waste acid resource.
(4) accompanying drawing explanation
Fig. 1 is nitrated operation spent acid comprehensive utilization process schema in reduzate production process.
(5) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
96% sulfuric acid 225g is added in the there-necked flask of 250ml, open and stir, add p acetamidoanisol 60g again, stirring makes raw material all dissolve in 2 hours, be cooled to 5 DEG C, start to drip nitric acid 22.9g (folding hundred), during dropping, temperature controls at 5-10 DEG C, insulated and stirred 1 hour again after nitric acid adds.After insulation terminates, nitrification liquid is slowly joined and is equipped with in the 1000ml beaker of 500g frozen water, be incubated 30min again after having diluted, filtering separation, obtain itrated compound filter cake and nitrating wasting acid mother liquor.
The itrated compound filter cake obtained washes filter with water to neutral (pH=6 ~ 7), obtains yellowish green wet product solid.Put into baking oven dry, calculated yield purity assay.Itrated compound purity is 98.92%, and yield is 94.04%.
The nitrating wasting acid mother liquor 650g (wherein sulfuric acid 29.55%, organism 0.41%) obtained joins in 1000ml flask, opens and stirs, slowly pass into ammonia and carry out neutralization reaction, be about 6.5, obtain neutralizer to solution ph.Then neutralizer is cooled to 20 DEG C, filtering separation, obtain organism precipitation and in and mother liquor.Organism precipitation drying, is weighed as 2.54 grams, reclaims and be used as nitrated raw material; In and add in mother liquor 653g (3% moisture evaporation) gac 2g (add-on be in and mother liquor amount 0.3%) decolour, and then carry out MVR evaporation concentration, obtain ammonia sulfate crystal 258g, nitrogen content >=21%, reach industrial sulphuric acid ammonium standard.Concentrated recycling condensing water is in the nitrated filter cake of washing.
Embodiment 2:
96% sulfuric acid 250g is added in the there-necked flask of 250ml, open and stir, add the organism 2.54g of p acetamidoanisol 60g and embodiment 1 recovery again, stirring makes raw material all dissolve in 2 hours, be cooled to 5 DEG C, start to drip nitric acid 23.2g (folding hundred), during dropping, temperature controls at 5 ~ 10 DEG C, insulated and stirred 1 hour again after nitric acid adds.After insulation terminates, nitrification liquid is slowly joined and is equipped with in the 1000ml beaker of 550g frozen water, be incubated 30min again after having diluted, filtering separation, obtain itrated compound filter cake and nitrating wasting acid mother liquor.
The itrated compound filter cake obtained, be washed to neutrality (pH=6 ~ 7), compacting, obtains greenish yellow solid.Put into baking oven dry, calculated yield purity assay.Itrated compound purity is about 98.78%, and yield is at about 97.42% (higher than the yield of embodiment 1 3.38%).
The nitrating wasting acid mother liquor obtained, adding liquefied ammonia, to be neutralized to pH value be about 5.0, is cooled to 20 DEG C, filtering separation, obtain organism precipitation, in and mother liquor.Return as nitrated raw material after organism precipitation reclaims.
In and mother liquor in add gac (quality be in and mother liquor 0.3%) decolouring, bleaching temperature controls at 30 ~ 35 DEG C, insulated and stirred 1 ~ 2 hour, reaction terminates the active breeze of rear filtering, filtrate adds 30% (w/w) hydrogen peroxide again and is oxidized, hydrogen peroxide add quality (folding hundred amounts) be in 0.15% of mother liquor quality, oxidizing temperature controls at 30 ~ 35 DEG C, oxidization time is 1.5 hours, after oxidation, solution is through concentrated, crystallization, separation obtains ammonium sulfate wet product, obtain ammonium sulfate finished product after drying, nitrogen content >=21%, reach industrial sulphuric acid ammonium standard.Concentrated recycling condensing water is in the nitrated filter cake of washing.
Embodiment 3:
96% sulfuric acid 250g is added in the there-necked flask of 250ml, open and stir, add the organism 2.54g of p acetamidoanisol 60g and embodiment 1 recovery again, stirring makes raw material all dissolve in 2 hours, be cooled to 5 DEG C, start to drip nitric acid 23.2g (folding hundred), during dropping, temperature controls at 5 ~ 10 DEG C, insulated and stirred 1 hour again after nitric acid adds.After insulation terminates, nitrification liquid is slowly joined and is equipped with in the 1000ml beaker of 550g frozen water, be incubated 30min again after having diluted, filtering separation, obtain itrated compound filter cake and nitrating wasting acid mother liquor.
The nitrating wasting acid mother liquor obtained, adding liquefied ammonia, to be neutralized to pH value be 5.0, is cooled to 20 DEG C, filtering separation, obtain organism precipitation, in and mother liquor.Return as nitrated raw material after organism precipitation reclaims.
In and mother liquor in add gac (quality be in and mother liquor 0.3%) decolouring, bleaching temperature controls at 30 ~ 35 DEG C, insulated and stirred 1 ~ 2 hour, reaction terminates the active breeze of rear filtering, pass into the ozonized air (namely containing the air of ozone 1%) that concentration is 1% (v/v) to be again oxidized, wherein ozone add quality (folding hundred amounts) be in 0.05% of mother liquor quality, oxidizing temperature controls at 30 ~ 35 DEG C, oxidization time is 1 hour, after oxidation, solution is through concentrated, crystallization, separation obtains ammonium sulfate wet product, obtain ammonium sulfate finished product after drying, nitrogen content >=21%, reach industrial sulphuric acid ammonium standard.Concentrated recycling condensing water is in the nitrated filter cake of washing.
Embodiment 4:
96% sulfuric acid 250g is added in the there-necked flask of 250ml, open and stir, add the organism 2.54g of p acetamidoanisol 60g and embodiment 1 recovery again, stirring makes raw material all dissolve in 2 hours, be cooled to 5 DEG C, start to drip nitric acid 23.2g (folding hundred), during dropping, temperature controls at 5 ~ 10 DEG C, insulated and stirred 1 hour again after nitric acid adds.After insulation terminates, nitrification liquid is slowly joined and is equipped with in the 1000ml beaker of 550g frozen water, be incubated 30min again after having diluted, filtering separation, obtain itrated compound filter cake and nitrating wasting acid mother liquor.
The nitrating wasting acid mother liquor obtained, adding liquefied ammonia, to be neutralized to pH value be 5.5, is cooled to 20 DEG C, filtering separation, obtain organism precipitation, in and mother liquor.Return as nitrated raw material after organism precipitation reclaims.
In and the hydrogen peroxide that adds 30% (w/w) in mother liquor be oxidized, hydrogen peroxide quality (folding hundred amounts) be in 0.5% of mother liquor quality, oxidizing temperature controls at 30 ~ 35 DEG C, oxidization time is 1.5 hours, solution after oxidation add again quality be in and the activated carbon decolorizing of mother liquor quality 0.2%, bleaching temperature controls at 30 ~ 35 DEG C, insulated and stirred 45 minutes, the active breeze of filtering, concentrating filter liquor, crystallization, separation obtain ammonium sulfate wet product, obtain ammonium sulfate finished product after drying.Nitrogen content >=21%, reaches industrial sulphuric acid ammonium standard.Concentrated recycling condensing water is in the nitrated filter cake of washing.
Claims (2)
1. a recoverying and utilizing method for nitrating wasting acid, described method comprises:
(1) spent acid neutralization: collect p acetamidoanisol and the reacted nitrating wasting acid mother liquor of nitration mixture, passes into ammonia or adds liquefied ammonia that to be neutralized to pH value be 5 ~ 7 under stirring, obtain neutralizer;
(2) separating organic matters: the neutralizer of step (1) is cooled to 20 ~ 40 DEG C, separates out solid through press filtration or centrifugation, returns as nitrated operation raw material after recovery, and residue neutralizer carries out next step operation;
(3) purification and impurity removal: step (2) residue neutralizer carries out purification and impurity removal with activated carbon decolorizing or activated carbon decolorizing with the oxidizing mode of combining, described activated carbon decolorizing is for adding gac insulated and stirred 0.25 ~ 2 hour at 20 DEG C ~ 50 DEG C, described oxidizing for adding oxygenant insulated and stirred 0.25 ~ 2 hour at 20 ~ 35 DEG C;
(4) condensing crystal: the neutralizer in step (3) after purification and impurity removal, through concentrated, crystallization, obtains solid ammonium sulfate, recycling condensing water.
2. the method for claim 1, it is characterized in that oxygenant in described step (3) is one of following or wherein two or more mixture: clorox, hydrogen peroxide, dioxide peroxide, ozone, its quality consumption is 0.02% ~ 1% of described neutralizer quality; Described quality of activated carbon consumption be described in and liquid measure 0.05% ~ 2%.
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| CN104098215B (en) * | 2014-07-31 | 2015-12-09 | 广西田东达盛化工科技有限公司 | The treatment process of acid waste water in 2-ethyl-anthraquinone production process |
| CN105858627B (en) * | 2016-05-06 | 2018-02-23 | 衢州学院 | The recovery method of benzene homologues nitrating wasting acid |
| CN109796342A (en) * | 2018-12-28 | 2019-05-24 | 阜宁县安勤化学有限公司 | A kind of waste acid treatment method that m-nitroacetophenone is synthetically produced |
| CN109851127A (en) * | 2019-02-01 | 2019-06-07 | 山东世纪阳光科技有限公司 | A kind of processing method of large red-based g spent acid |
| CN110511146A (en) * | 2019-09-17 | 2019-11-29 | 四川北方红光特种化工有限公司 | The production method and its production system of a kind of low single nitro ortho-xylene of waste acid quantity |
| CN110950312A (en) * | 2019-12-19 | 2020-04-03 | 天门楚天生物科技有限公司 | Method for comprehensively treating primary nitrification mother liquor and secondary nitrification mother liquor |
| CN111792997B (en) * | 2020-07-17 | 2023-03-24 | 四川北方红光特种化工有限公司 | Process method for improving waste acid curing |
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Effective date of registration: 20170825 Address after: 312369 weft three road, Shangyu Industrial Park, Hangzhou, Zhejiang Co-patentee after: SHANGHAI HONGYUAN XINCHUANG MATERIAL TECHNOLOGY CO., LTD. Patentee after: Zhejiang Hongsheng Chemical Research Limited Co-patentee after: Zhejiang Longsheng Chemicals Co., Ltd. Address before: Hangzhou Bay Industrial Park three weft road 312369 Zhejiang province Shaoxing City, Shangyu City, No. 15 Patentee before: Zhejiang Longsheng Chemicals Co., Ltd. |