CN105669500A - Method adopting clean process for preparing H-acid - Google Patents
Method adopting clean process for preparing H-acid Download PDFInfo
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- CN105669500A CN105669500A CN201610112769.1A CN201610112769A CN105669500A CN 105669500 A CN105669500 A CN 105669500A CN 201610112769 A CN201610112769 A CN 201610112769A CN 105669500 A CN105669500 A CN 105669500A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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Abstract
The invention discloses a method adopting a clean process for preparing H-acid. The method comprises the following process: step (10), carrying out extraction treatment on denitrated matter to obtain dilute sulphuric acid and an extracted mixture, and carrying out re-extraction on the extracted mixture to obtain a nitro-T-acid solution; step (20), carrying out reduction treatment on the nitro-T-acid solution obtained in the step (10) to obtain an amino-T-acid solution; step (30), respectively carrying out concentration treatment on the amino-T-acid solution obtained in the step (20) and caustic soda liquid to obtain concentrated amino-T-acid solution and caustic soda liquid; step (40), carrying out alkali fusion treatment on the concentrated amino-T-acid solution and caustic soda liquid obtained in the step (30), and performing attenuation treatment to obtain attenuated alkali fusion matter; step (50), carrying out separation and filtration treatment on the attenuated alkali fusion matter obtained in the step (40) to obtain the H-acid. The preparation method disclosed by the invention adopts the clean process for preparing the H-acid, the production efficiency is high, the materials are saved, and the economic cost is reduced.
Description
Technical field
The present invention relates to the preparation field of dye material, it particularly relates to a kind of method adopting cleaning procedure to prepare H-acid.
Background technology
H-acid is the important source material of dye industry, mainly for the production of reactive dye, direct dyes, acid stain, it is also possible to be used for producing the products such as chromotropic acid. The chemical name of H-acid is: 1-amino-8-naphthol-3,6-disulfonic acid. The chemical structural formula of H-acid is:
The molecular formula of H-acid: C10H9NO7S2, relative molecular mass: 319.3. H-acid dry product is white to gray crystals powder. It is slightly soluble in cold water, is soluble in hot water, be dissolved in the alkaline solution such as soda or Caustic soda, be reddish brown purple with ferric chloride effect, be dissolved in alkaline solution dark green.
H-processed with acid is made with a long history, but is still most important intermediate in naphthalene system so far. Current domestic production H-acid mainly adopts batch process. Batch process produces technique that H-acid adopts with refined naphthalene for main material, is prepared by sulfonation, nitrated, denitration, neutralization, reduction, filter pressing, isolation, filtration, dissolving, alkali fusion, isolation, filtration, drying and other steps. Production process is based on intermittently operated, and process route is longer, and production capacity is low, and yield is relatively low, and three wastes discharge amount is big. Domestic existing this process route commonly used.
Summary of the invention
Technical problem: the technical problem to be solved is: provide a kind of method adopting cleaning procedure to prepare H-acid, this preparation method adopts cleaning procedure to make H-acid, and production efficiency is high, saves material, reduces Financial cost.
Technical scheme: for solving above-mentioned technical problem, the technical scheme that the embodiment of the present invention adopts is:
A kind of method adopting cleaning procedure to prepare H-acid, described method includes procedure below:
Step 10) denitration thing is carried out extraction process, obtain dilute sulfuric acid and extract mixture, and carrying out back extraction to extracting mixture, obtaining nitrobased NPK solution;
Step 20) to step 10) obtain nitrobased NPK solution and carry out reduction treatment, obtain amino T acid solution;
Step 30) to step 20) obtain amino T acid solution and liquid caustic soda carries out concentration respectively, amino T acid solution after being concentrated and liquid caustic soda;
Step 40) to step 30) amino T acid solution after the concentration that obtains and liquid caustic soda carry out alkali fusion process, and be diluted processing, the alkali fusion thing after being diluted;
Step 50) to step 40) alkali fusion thing after the dilution that obtains, carry out isolating and filtration treatment, obtain H-acid.
As preference, described step 10) specifically include: denitration thing, extractant and water are continuously pumped into extraction reactor, after four-stage counter-current extractive reaction, are extracted mixture and dilute sulfuric acid; Dilute sulfuric acid is cooled, activated carbon adsorption is stored in the first dilute sulfuric acid surge tank after processing; Extraction mixture liquid caustic soda is carried out back extraction in back extraction reactor, it is extracted agent and nitrobased NPK solution, extractant is returned in extraction reactor, carry out extractive reaction, and after cooled for nitrobased NPK solution, activated carbon adsorption are processed, deliver in nitrobased NPK storage tank.
As preference, described step 20) specifically include: after catalyst, hydrogen, the preheating of nitrobased NPK solution, deliver in hydrogenation reactor, carrying out hydrogenation reduction, material is cooled to 90 DEG C with water after terminating by reaction, obtaining reactant mixture, hot water is for lower step amino T acid preheating; By reactant mixture through gas-liquid separator separates, and after release, obtain amino T acid solution and catalyst, amino T acid solution is delivered in amino T acid storage tank; Utilize filtration system to reclaim catalyst, and the catalyst of recovery is recycled and reused in hydrogenation reactor.
As preference, the described temperature carrying out hydrogenation reduction is 170 DEG C, and pressure is 20Mpa.
As preference, described step 30) specifically include: utilize step 20) in the hot water that obtains when being cooled to 90 DEG C of material, amino T acid solution is preheated, imitates adverse currents through 5 and be concentrated into setting concentration, be then sent in dense T acid buffering tank; Liquid caustic soda is imitated adverse current through 2 and is concentrated into the liquid caustic soda that mass concentration is 72%, be then sent in dope alkali surge tank.
As preference, described step 40) specifically include: by step 30) concentration after liquid caustic soda be preheated to 180 DEG C through heat exchanger, it is then fed in alkali-melting vessel, alkali-melting vessel is pumped into after being preheated respectively by amino T acid solution after methanol and concentration subsequently, liquid caustic soda, methanol and amino T acid solution react, after reaction terminates, by dilute in material press-in dilution still, obtain the alkali fusion thing after dilute methanol and dilution; The dilute methanol steamed is reclaimed in condensation, and the alkali fusion thing after dilution reclaims residual methanol through stripper; Dilute methanol is delivered to methanol rectification workshop section and reclaims methanol, and the methanol of recovery is used in alkali fusion reaction next time; Alkali fusion thing after dilution is sent in alkali fusion thing surge tank.
As preference, the temperature that described liquid caustic soda, methanol and amino T acid solution react is 200 DEG C, and pressure is 2.8Mpa.
As preference, described step 50) specifically include:
Carry out complex acid process: by step 10) dilute sulfuric acid that obtains, mix with the sulphuric acid that mass concentration is 98%, cool down, be made into the dilute sulfuric acid setting concentration, and send in the second dilute sulfuric acid surge tank;
Carry out isolation process: by step 40) the alkali fusion thing after dilution, the dilute sulfuric acid in H-acid washing water and the second dilute sulfuric acid surge tank, deliver to and separation kettle carry out isolation process, the sulfur dioxide of generation after cooling, reclaim by liquefaction;
Carrying out cooling down and filtration treatment: by the material after isolation processes, cooled still continuous coo1ing, to 50 DEG C, filters with filter, washes, obtain H-acidleach cake, wash water and mother solution, be stored in by wash water in wash water tank, process for isolation next time;Mother solution is delivered in Waste Water Treatment.
Beneficial effect: compared with prior art, the embodiment of the present invention has the advantages that above-described embodiment prepares H-acid through extraction, hydrogenating reduction, concentration, alkali fusion, isolation, filtration, drying and other steps, whole technique serialization, substantially increases production efficiency. Simultaneously in preparation process, part material is reclaimed, recycling, greatly reduce Financial cost.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is described in detail.
A kind of method adopting cleaning procedure to prepare H-acid of the embodiment of the present invention, including procedure below:
Step 10) denitration thing is carried out extraction process, obtain dilute sulfuric acid and extract mixture, and carrying out back extraction to extracting mixture, obtaining nitrobased NPK solution;
Step 20) to step 10) obtain nitrobased NPK solution and carry out reduction treatment, obtain amino T acid solution;
Step 30) to step 20) obtain amino T acid solution and liquid caustic soda carries out concentration respectively, amino T acid solution after being concentrated and liquid caustic soda;
Step 40) to step 30) amino T acid solution after the concentration that obtains and liquid caustic soda carry out alkali fusion process, and be diluted processing, the alkali fusion thing after being diluted;
Step 50) to step 40) alkali fusion thing after the dilution that obtains, carry out isolating and filtration treatment, obtain H-acid.
Above-described embodiment prepares H-acid, whole technique serialization through steps such as extraction, hydrogenating reduction, concentration, alkali fusion, isolation, filtrations. Adopt closed reaction simultaneously, reduce the uncontrollable discharge of waste gas and waste liquid.
The present embodiment adopts solvent extraction technology to replace crude salt analysis technique, has not only saved a large amount of neutralization ammonia, and has decreased the generation of T-acid isolation waste water. What extraction produced dilute sulfuric acid can be additionally used in H-acid isolation procedures, and the sulphuric acid decreasing H-acid isolation makes consumption; Only this step can make yield improve about 10%, saves substantial amounts of resource consumption simultaneously. The present embodiment adopts hydrogenating reduction clearer production technology to replace iron powder reducing, and product yield improves about 3%, thoroughly eliminates the generation of iron cement, can reduce the generation of more than about 60,000 tons iron cements every year.
Preferably, described step 10) specifically include: denitration thing, extractant and water are continuously pumped into extraction reactor, after four-stage counter-current extractive reaction, are extracted mixture and dilute sulfuric acid; Dilute sulfuric acid is cooled, activated carbon adsorption is stored in the first dilute sulfuric acid surge tank after processing; Extraction mixture liquid caustic soda is carried out back extraction in back extraction reactor, it is extracted agent and nitrobased NPK solution, extractant is returned in extraction reactor, carry out extractive reaction, and after cooled for nitrobased NPK solution, activated carbon adsorption are processed, deliver in nitrobased NPK storage tank.
In this step, TEHA selected by extractant, and molecular formula formula is: C24H51N. Step 10) extraction process and back extraction process chemical equation be expressed as follows:
In this step, after carrying out back extraction process, the extractant generated is returned in extraction reactor, carries out extractive reaction. Thus it is greatly saved in extractive reaction process the extractant quantity needed so that extractant is in the process producing H-acid continuously, it is possible to reuses, reduces cost.
Preferably, described step 20) specifically include: after catalyst, hydrogen, the preheating of nitrobased NPK solution, deliver in hydrogenation reactor, 170 DEG C, carry out hydrogenation reduction under 20MPa, after reaction terminates, with water, material being cooled to 90 DEG C, obtain reactant mixture, hot water is for lower step amino T acid preheating;By reactant mixture through gas-liquid separator separates, and after release, obtain amino T acid solution and catalyst, amino T acid solution is delivered in amino T acid storage tank; Utilize filtration system to reclaim catalyst, and the catalyst of recovery is recycled and reused in hydrogenation reactor.
In this preference, as preferably, catalyst is Raney's nickel. Step 20) it is expressed as follows with chemical equation:
In this step, after material being cooled to 90 DEG C with water, water becomes hot water, it is possible to preheat for amino T acid in subsequent step. So be conducive to saving heat energy source. It addition, utilize filtration system to reclaim catalyst, and the catalyst of recovery is recycled and reused in hydrogenation reactor, in the process producing H-acid continuously, makes full use of existing material, and reused, advantageously reduce cost.
Preferably, described step 30) specifically include: utilize step 20) in the hot water that obtains when being cooled to 90 DEG C of material, amino T acid solution is preheated, imitates adverse currents through 5 and be concentrated into setting concentration, be then sent in dense T acid buffering tank;
Liquid caustic soda is imitated adverse current through 2 and is concentrated into the liquid caustic soda that mass concentration is 72%, be then sent in dope alkali surge tank.
Preferably, described step 40) specifically include: by step 30) concentration after liquid caustic soda be preheated to 180 DEG C through heat exchanger, it is then fed in alkali-melting vessel, alkali-melting vessel is pumped into after being preheated respectively by amino T acid solution after methanol and concentration subsequently, liquid caustic soda, methanol and amino T acid solution 200 DEG C, react under 2.8MPa, after reaction terminates, by dilute in material press-in dilution still, obtain the alkali fusion thing after dilute methanol and dilution; The dilute methanol steamed is reclaimed in condensation, and the alkali fusion thing after dilution reclaims residual methanol through stripper; Dilute methanol is delivered to methanol rectification workshop section and reclaims methanol, and the methanol of recovery is used in alkali fusion reaction next time; Alkali fusion thing after dilution is sent in alkali fusion thing surge tank.
In this step, reacted dilute methanol is reclaimed, and be used for alkali fusion reaction next time by reclaiming the dilute methanol obtained. Recycling of methanol solution, greatly reduces and generates quantity of methyl alcohol required in H-acid process, advantageously reduce cost.
Step 40) it is expressed as follows with chemical equation:
Preferably, described step 50) specifically include:
Carry out complex acid process: by step 10) dilute sulfuric acid that obtains, mix with the sulphuric acid that mass concentration is 98%, cool down, be made into the dilute sulfuric acid setting concentration, and send in the second dilute sulfuric acid surge tank;
Carry out isolation process: by step 40) the alkali fusion thing after dilution, the dilute sulfuric acid in H-acid washing water and the second dilute sulfuric acid surge tank, deliver to and separation kettle carry out isolation process, the sulfur dioxide of generation after cooling, reclaim by liquefaction.
Carrying out cooling down and filtration treatment: by the material after isolation processes, cooled still continuous coo1ing, to 50 DEG C, filters with filter, washes, obtain H-acidleach cake, wash water and mother solution, be stored in by wash water in wash water tank, process for isolation next time; Mother solution is delivered in Waste Water Treatment.
In this step, by step 10) dilute sulfuric acid that obtains for, in this step, improve the utilization rate of dilute sulfuric acid, be conducive to saving cost. Step 50) it is expressed as follows with chemical equation:
H2SO4+2NaOH→Na2SO4+2H2O
H2SO4+Na2SO3→Na2SO4+SO2+H2O
By step 50) prepare after H-acid, it is possible to H-acid in spin flash dryer with hot air drying, dry tail gas enters air after cyclonic separation, bag-type dust; The H-acid finished product obtained, is then fed into subsequent packages operation.
In the above-described embodiments, step 10) in denitration thing through liquid naphthalene being carried out sulfonation, nitrated and denitration obtains after processing. Specifically include:
Sulfonation processes: liquid naphthalene and the sulfuric acid solution that mass concentration is 100% are continuously added in sulphonation kettle, temperature in sulphonation kettle is upgraded to 90 DEG C, carry out first time sulfonation, it is continuously introduced in transposition sulfonation tower by after the buffered tank of product after first time sulfonation, temperature in transposition sulfonation tower is upgraded to 150 DEG C, carries out translocation reaction;
Material that translocation reaction is completed, mass concentration be 100% sulfuric acid solution and oleum that mass concentration is 65% be continuously introduced in sulfonation reactor, the temperature in sulfonation reactor is 65 DEG C, carries out second time sulfonation;
Three sulfonation towers delivered to by material and the oleum that mass concentration is 65% after second time sulfonation being completed, and the temperature in three sulfonation towers is upgraded to 150 DEG C, carry out third time sulfonation, generate sulfonated bodies, and sulfonated bodies is sent into storage in sulfonated bodies surge tank. Sulfonated bodies is that nitration treatment is standby.
Sulfonation process chemical equation is expressed as follows:
The preparation of liquid naphthalene can adopt following method: after solid refined naphthalene steam adds heat fusing, after filtering out impurities, makes liquid naphthalene.
Nitration treatment: by step 10) prepare sulfonated bodies and the nitric acid that mass concentration is 68% be continuously pumped in one-level nitrator, and cooling water-cooled but under nitrated in 40 DEG C, then overflow is to two grades of nitrating pots, complete nitration reaction, the itrated compound generated after reaction is sent into storage in itrated compound surge tank. Step 20) it is expressed as follows with chemical equation:
Denitration processes: squeeze in Benitration reactor with pump by water, simultaneously by step 20) itrated compound for preparing flows into Benitration reactor, homogeneous mixture of material, and generate denitration thing, after cooling, send in denitration thing surge tank through denitration thing. The nitrogen oxide gas produced in denitration reaction process, condensed rear alkali liquor, for instance sodium hydroxide absorbs, and enters air after reaching standard.
2HNO3→NO2+NO+O2+H2O
NO2+NO+2NaOH→2NaNO2+H2O
The ultimate principle of the present invention, principal character and advantage have more than been shown and described. Skilled person will appreciate that; the present invention is not by the restriction of above-mentioned specific embodiment; description in above-mentioned specific embodiment and description is intended merely to and further illustrates principles of the invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention. The scope of protection of present invention is defined by claims and equivalent thereof.
Claims (10)
1. one kind adopts the method that cleaning procedure prepares H-acid, it is characterised in that described method includes procedure below:
Step 10) denitration thing is carried out extraction process, obtain dilute sulfuric acid and extract mixture, and carrying out back extraction to extracting mixture, obtaining nitrobased NPK solution;
Step 20) to step 10) obtain nitrobased NPK solution and carry out reduction treatment, obtain amino T acid solution;
Step 30) to step 20) obtain amino T acid solution and liquid caustic soda carries out concentration respectively, amino T acid solution after being concentrated and liquid caustic soda;
Step 40) to step 30) amino T acid solution after the concentration that obtains and liquid caustic soda carry out alkali fusion process, and be diluted processing, the alkali fusion thing after being diluted;
Step 50) to step 40) alkali fusion thing after the dilution that obtains, carry out isolating and filtration treatment, obtain H-acid.
2. the cleaning procedure that adopts described in claim 1 prepares the sour method of H-, it is characterized in that, described step 10) specifically include: denitration thing, extractant and water are continuously pumped into extraction reactor, after four-stage counter-current extractive reaction, are extracted mixture and dilute sulfuric acid;Dilute sulfuric acid is cooled, activated carbon adsorption is stored in the first dilute sulfuric acid surge tank after processing; Extraction mixture liquid caustic soda is carried out back extraction in back extraction reactor, it is extracted agent and nitrobased NPK solution, extractant is returned in extraction reactor, carry out extractive reaction, and after cooled for nitrobased NPK solution, activated carbon adsorption are processed, deliver in nitrobased NPK storage tank.
3. the cleaning procedure that adopts described in claim 1 prepares the sour method of H-, it is characterised in that described extractant molecules formula formula is: C24H51N。
4. the cleaning procedure that adopts described in claim 1 prepares the sour method of H-, it is characterized in that, described step 20) specifically include: after catalyst, hydrogen, the preheating of nitrobased NPK solution, deliver in hydrogenation reactor, carrying out hydrogenation reduction, material is cooled to 90 DEG C with water after terminating by reaction, obtaining reactant mixture, hot water is for lower step amino T acid preheating; By reactant mixture through gas-liquid separator separates, and after release, obtain amino T acid solution and catalyst, amino T acid solution is delivered in amino T acid storage tank; Utilize filtration system to reclaim catalyst, and the catalyst of recovery is recycled and reused in hydrogenation reactor.
5. the cleaning procedure that adopts described in claim 4 prepares the sour method of H-, it is characterised in that described catalyst is Raney's nickel.
6. the cleaning procedure that adopts described in claim 4 prepares the sour method of H-, it is characterised in that the described temperature carrying out hydrogenation reduction is 170 DEG C, and pressure is 20Mpa.
7. the cleaning procedure that adopts described in claim 4 prepares the sour method of H-, it is characterised in that described step 30) specifically include:
Utilize step 20) in the hot water that obtains when being cooled to 90 DEG C of material, amino T acid solution is preheated, imitates adverse currents through 5 and be concentrated into setting concentration, be then sent in dense T acid buffering tank;
Liquid caustic soda is imitated adverse current through 2 and is concentrated into the liquid caustic soda that mass concentration is 72%, be then sent in dope alkali surge tank.
8. the cleaning procedure that adopts described in claim 1 prepares the sour method of H-, it is characterized in that, described step 40) specifically include: by step 30) concentration after liquid caustic soda be preheated to 180 DEG C through heat exchanger, it is then fed in alkali-melting vessel, pumping into alkali-melting vessel after being preheated respectively by amino T acid solution after methanol and concentration subsequently, liquid caustic soda, methanol and amino T acid solution react, after reaction terminates, by dilute in material press-in dilution still, obtain the alkali fusion thing after dilute methanol and dilution; The dilute methanol steamed is reclaimed in condensation, and the alkali fusion thing after dilution reclaims residual methanol through stripper; Dilute methanol is delivered to methanol rectification workshop section and reclaims methanol, and the methanol of recovery is used in alkali fusion reaction next time; Alkali fusion thing after dilution is sent in alkali fusion thing surge tank.
9. adopt, described in claim 1, the method that cleaning procedure prepares H-acid, it is characterised in that the temperature that described liquid caustic soda, methanol and amino T acid solution react is 200 DEG C, and pressure is 2.8Mpa.
10. the cleaning procedure that adopts described in claim 1 prepares the sour method of H-, it is characterised in that described step 50) specifically include:
Carry out complex acid process: by step 10) dilute sulfuric acid that obtains, mix with the sulphuric acid that mass concentration is 98%, cool down, be made into the dilute sulfuric acid setting concentration, and send in the second dilute sulfuric acid surge tank;
Carry out isolation process: by step 40) the alkali fusion thing after dilution, the dilute sulfuric acid in H-acid washing water and the second dilute sulfuric acid surge tank, deliver to and separation kettle carry out isolation process, the sulfur dioxide of generation after cooling, reclaim by liquefaction;
Carrying out cooling down and filtration treatment: by the material after isolation processes, cooled still continuous coo1ing, to 50 DEG C, filters with filter, washes, obtain H-acidleach cake, wash water and mother solution, be stored in by wash water in wash water tank, process for isolation next time; Mother solution is delivered in Waste Water Treatment.
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| CN108003070A (en) * | 2017-12-22 | 2018-05-08 | 绍兴杰派化工科技有限公司 | A kind of method of sulfonation in H acid production |
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| WO2020052577A1 (en) * | 2018-09-13 | 2020-03-19 | 山东创蓝垚石环保技术有限公司 | Process for producing h acid by recycling alkali fusion mother liquor |
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Application publication date: 20160615 |