CN105152142A - Method for recovering sulfuric acid from waste acid produced by anthraquinone production - Google Patents
Method for recovering sulfuric acid from waste acid produced by anthraquinone production Download PDFInfo
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- CN105152142A CN105152142A CN201510294939.8A CN201510294939A CN105152142A CN 105152142 A CN105152142 A CN 105152142A CN 201510294939 A CN201510294939 A CN 201510294939A CN 105152142 A CN105152142 A CN 105152142A
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Abstract
The invention discloses a method for recovering sulfuric acid from waste acid produced by anthraquinone production. The method comprises carrying out solid-liquid separation on anthraquinone waste acid, adding active carbon into the separated waste acid solution, carrying out solid-liquid separation, carrying out vacuum concentration on the waste acid filtrate to obtain a concentrated solution with a sulfuric acid mass fraction of 90% or more, adding a nitric acid solution into the concentrated solution, and carrying out oxidation until the concentrated solution is clear and transparent. Through adsorption, condensation and oxidation, a sulfuric acid component is recovered from anthraquinone waste acid. The method utilizes easily available raw materials and process control is easy.
Description
Technical field
The present invention relates to the treatment process producing spent acid in a kind of anthraquinone production process, the New Process for Treatment of particularly a kind of anthraquinone waste acid concentration, decolouring, recovery.
Background technology
Sulfuric acid has a large amount of application in anthraquinone production process.In anthraquinone is produced, the utilization ratio of sulfuric acid is lower, and a large amount of spent acid is got rid of outward along with spent acid.These spent acid not only cause the acidifying in soil also to waste sulfuric acid resource greatly outward after arranging, Treatment process advanced thus also develops rapidly.Recognize according to the patent of having consulted and periodical literature, the process of anthraquinone spent acid mainly contains following several means: 1, extracting sulfuric acid salt method.In Chinese patent CN201410504121.X, Yi Keli environmental protection development in science and technology company limited and Institutes Of Technology Of Tianjin utilize the sulfuric acid component in anthraquinone spent acid, adopt absorption, oxidation, neutralizing treatment technique, obtain magnesium sulfate finished product.Thus while process anthraquinone spent acid, obtain magnesium sulfate product.This kind for the treatment of process, although can reclaim(ed) sulfuric acid component, products obtained therefrom added value be lower, and processing cost accompanies higher.And in treating processes, the moisture in spent acid is brought in magnesium sulfate product, causes secondary topsoil in drying process.2, oxidation style.Wu Changlong, Chen Jinlong mentions in " improvement of Waste Sulfuric Acid and sulfur acid waste water ", Tianjin seven material eight factory adopts nitric acid to be that oxygenant carries out oxide treatment to anthraquinone nitrating wasting acid, its operating process is: spent acid being diluted to sulfuric acid content is 30%, that contained dinitroanthraquinone is separated out to greatest extent, after filter pocket vacuum filtration, spent acid enters and rises film shell and tube evaporator and carry out being concentrated into sulfuric acid content 70%, take water vapour out of with squirt pump again and reach 93% to sulfuric acid content, then flow in enamel stills for air blowing, add nitric acid and carry out oxide treatment, be light yellow to sulfuric acid, the oxynitride alkali liquor absorption produced in reaction.This method can reclaim and obtain comparatively pure sulphuric acid soln, but nitric acid consumption is higher, and concentration operation is loaded down with trivial details.3, directly usage is overlapped.Chen Yunshi mentions in " the waste acid water cover in the production of 1.4-dihydroxyanthraquinone is used for the experimental study of hydroquinone oxidation technique ", anthraquinone spent acid is filtered and filters after crystallisation by cooling and isolate hydroxyl in spent acid and phthalic acid respectively, then normality is mixed with industrial sulphuric acid, cover is used for the oxidizing process of dihydroxy-benzene, test apply mechanically sulfuric acid compared with industrial sulphuric acid, yield differs 1 percentage point.As can be seen here, although yield is substantially suitable, but differentiated, and not separated impurity, in recycled process, easily cause inrichment, have considerable influence to quality product.4, fenton oxidation style.Company limited of chemical research designing institute mentioned and adopted fenton reagent oxidation process anthraquinone spent acid solution in " in alkyl-anthraquinone production process spent acid process and the utilization " delivered dawn, then with aluminium hydroxide neutralization, made Tai-Ace S 150 product.But containing a large amount of iron ions in products obtained therefrom, need to carry out flocculation treatment and just can reach product standard, complicated operation, and added value of product is lower.
Summary of the invention
Object of the present invention is exactly for above-mentioned the deficiencies in the prior art, provides a kind of method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process that treatment process controls simply, starting material are easy to get.
The technical solution used in the present invention is as follows:
A kind of method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process, it is characterized in that its method steps is as follows: first anthraquinone spent acid is carried out solid-liquid separation, gac is added in the waste acid liquor obtained after isolation again, again carry out solid-liquid separation afterwards, the spent acid filtrate obtained is carried out vacuum concentration again and is obtained the concentrated solution of sulfuric acid massfraction more than 90%, adds salpeter solution and carry out being oxidizing to concentrated solution and reach clear in the concentrated solution after concentrated.
Described anthraquinone spent acid is the solution of sulfuric acid massfraction 30-60%.
The weight ratio of described gac and waste acid liquor is at 2-3%.
Described charcoal absorption temperature is at 50-90 DEG C.
During described vacuum concentration, absolute pressure is 7-8kpa, temperature 180-200 DEG C.
Described salpeter solution is the aqueous nitric acid of massfraction 65%, and during oxidation, temperature is 160-220 DEG C.
The invention has the beneficial effects as follows:
In anthraquinone spent acid, main moiety is sulfuric acid, water and organism, the principal element affecting sulphuric acid concentration recovery or sale is exactly the organism in spent acid, as long as the organism in removing spent acid, removed moisture by vacuum concentration and just can obtain the reclaim(ed) sulfuric acid of high-content.The present invention adopts absorption, mode that is concentrated and oxidation reclaims the sulfuric acid component obtained in anthraquinone spent acid, and the starting material of production are easy to get, and technology controlling and process is simple.Compared with prior art, the present invention does not change the sulfuric acid component neutralization in spent acid into sulfate product, and operation is relatively simple, and increases filtration, charcoal absorption operation before the oxidation, the consumption of nitric acid can be effectively reduced, for many methods are available when processing anthraquinone spent acid.
Accompanying drawing explanation
Fig. 1 is technological process block-diagram of the present invention.
In Fig. 1,1, strainer; 2, still is adsorbed; 3, strainer; 4, concentration kettle; 5, stills for air blowing; 6, vacuum pump; 7, absorption kettle.
Embodiment
Below in conjunction with specific embodiments and the drawings, the invention will be further described:
Charcoal absorption and nitric acid oxidation process anthraquinone spent acid is used: anthraquinone spent acid carries out strainer 1 and carries out solid-liquid separation, is separated by suspended substance in spent acid, obtains comparatively pure waste acid liquor under following method condition.Waste acid liquor adds the gac of its weight 3% after arriving absorption still 2 in waste acid liquor, unlatching stirring and heating, is warming up to 80 DEG C and stops heating, and stirring maintenance still temperature carried out solid-liquid separation by strainer 3 after 2 hours.Temperature during charcoal absorption is at 50 ~ 90 DEG C.Being separated through filter 3 the spent acid filtrate obtained delivers in concentration kettle 4, and under the vacuum condition of 700mmHg post, heating concentration kettle temperature to 180 ~ 200 DEG C, make the massfraction of concentrated solution sulfuric acid in concentration kettle 4 reach 90%.Slowly let out except the vacuum in concentration kettle 4, when still 4 internal pressure to be concentrated reaches under condition of normal pressure, concentrated solution enters stills for air blowing 5, now open stirring, and maintain stills for air blowing 5 still temperature between 180 ~ 200 DEG C, backward stills for air blowing 5 in gelled acid in add the salpeter solution that massfraction is 65%, to stills for air blowing 5, sulphuric acid soln reaches clear.The oxynitride produced in stills for air blowing 5 oxidising process enters in absorption kettle 7 and is absorbed by sodium hydroxide lye, emission-free outer row.
Other the undeclared part that the present invention relates to adopts prior art to be realized.
Claims (6)
1. one kind utilizes the method for the waste acidity recovery sulfuric acid produced in anthraquinone production process, it is characterized in that its method steps is as follows: first anthraquinone spent acid is carried out solid-liquid separation, gac is added in the waste acid liquor obtained after isolation again, again carry out solid-liquid separation afterwards, the spent acid filtrate obtained is carried out vacuum concentration again and is obtained the concentrated solution of sulfuric acid massfraction more than 90%, adds salpeter solution and carry out being oxidizing to concentrated solution and reach clear in the concentrated solution after concentrated.
2. the method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process according to claim 1, is characterized in that described anthraquinone spent acid is the solution of sulfuric acid massfraction 30-60%.
3. the method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process according to claim 1 and 2, is characterized in that the weight ratio of described gac and waste acid liquor is at 2-3%.
4. the method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process according to claim 3, is characterized in that described charcoal absorption temperature is at 50-90 DEG C.
5. the method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process according to claim 2, when it is characterized in that described vacuum concentration, absolute pressure is 7-8kpa, temperature 180-200 DEG C.
6. the method utilizing the waste acidity recovery sulfuric acid produced in anthraquinone production process according to claim 1, is characterized in that described salpeter solution is the aqueous nitric acid of massfraction 65%, and during oxidation, temperature is 160-220 DEG C.
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| CN201510294939.8A CN105152142A (en) | 2015-06-02 | 2015-06-02 | Method for recovering sulfuric acid from waste acid produced by anthraquinone production |
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| CN201510294939.8A CN105152142A (en) | 2015-06-02 | 2015-06-02 | Method for recovering sulfuric acid from waste acid produced by anthraquinone production |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923610A (en) * | 2016-05-09 | 2016-09-07 | 杭州中昊科技有限公司 | Novel process of acetylene purification and waste acid regeneration |
| CN114477250A (en) * | 2022-01-25 | 2022-05-13 | 重庆毂运科技有限公司 | Method for preparing magnesium sulfate by using anthraquinone waste acid |
| CN114804035A (en) * | 2022-03-30 | 2022-07-29 | 南京绿联环境科技发展有限公司 | Separation and purification process of waste sulfuric acid containing organic matters |
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| CN102079512A (en) * | 2010-11-29 | 2011-06-01 | 重庆大学 | Process for recovering sulfuric acid and sulfate from waste acid generated in preparation of titanium dioxide by using sulfuric acid method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923610A (en) * | 2016-05-09 | 2016-09-07 | 杭州中昊科技有限公司 | Novel process of acetylene purification and waste acid regeneration |
| CN105923610B (en) * | 2016-05-09 | 2018-06-12 | 杭州中昊科技有限公司 | Acetylene cleaning acid regeneration technique |
| CN114477250A (en) * | 2022-01-25 | 2022-05-13 | 重庆毂运科技有限公司 | Method for preparing magnesium sulfate by using anthraquinone waste acid |
| CN114477250B (en) * | 2022-01-25 | 2024-04-19 | 重庆毂运科技有限公司 | Method for preparing magnesium sulfate by utilizing anthraquinone waste acid |
| CN114804035A (en) * | 2022-03-30 | 2022-07-29 | 南京绿联环境科技发展有限公司 | Separation and purification process of waste sulfuric acid containing organic matters |
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Application publication date: 20151216 |