CN105753744A - Energy-saving H-acid preparation device - Google Patents
Energy-saving H-acid preparation device Download PDFInfo
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- CN105753744A CN105753744A CN201610113728.4A CN201610113728A CN105753744A CN 105753744 A CN105753744 A CN 105753744A CN 201610113728 A CN201610113728 A CN 201610113728A CN 105753744 A CN105753744 A CN 105753744A
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- 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
Abstract
The invention discloses an energy-saving H-acid preparation device. The device comprises an extraction device, a reduction device, a concentration device, a dilution device and a dissociation and filter device, wherein a first outlet of the extraction device is connected with an inlet of the reduction device, an outlet of the reduction device is connected with the concentration device, an outlet of the concentration device is connected with an inlet of the dilution device, an outlet of the dilution device is connected with a first inlet of the dissociation and filter device, and a second inlet of the dissociation and filter device is connected with a second outlet of the extraction device. According to the preparation device, H-acid is prepared by virtue of a continuous production method, so that the production efficiency is high, materials are saved, and the economic cost is lowered.
Description
Technical field
The present invention relates to the preparation field of dye material, it particularly relates to a kind of H-acid preparation facilities with energy-saving effect.
Background technology
H-acid is the important source material of dye industry, mainly for the production of reactive dye, direct dyes, acid dyes, 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 that white is 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 ash or caustic soda, be reddish brown purple with ferric trichloride effect, be dissolved in alkaline solution dark green.
H-acid manufactures with a long history, but is the most still most important intermediate in naphthalene system.Domestic production H-acid at present mainly uses batch process.Batch process produces technique that H-acid uses with refined naphthalene as main material, by sulfonation, nitrification, denitration, neutralize, reduce, press filtration, isolate, filter, dissolve, alkali fusion, isolate, filter, drying and other steps prepares.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 H-acid preparation facilities with energy-saving effect, this preparation facilities uses quantity-produced method 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 uses is:
A kind of H-acid preparation facilities with energy-saving effect, this device includes extraction equipment, reduction apparatus, enrichment facility, air mix facilities, isolation and filter, first outlet of extraction equipment is connected with the import of reduction apparatus, the outlet of reduction apparatus is connected with the import of enrichment facility, the outlet of enrichment facility is connected with the import of air mix facilities, the outlet of air mix facilities is connected with the first import of isolation and filter, and the second outlet of isolation and the second import of filter and extraction equipment connects.
Preferably, described extraction equipment includes the second pump, extraction reactor, the first cooling and absorbent charcoal adsorber, the first dilute sulfuric acid surge tank, back extraction reactor, the second cooling and absorbent charcoal adsorber, nitrobased NPK storage tank；The import of the second pump is connected with the outlet of denitration thing surge tank, second delivery side of pump is connected with the first import of extraction reactor, first outlet of extraction reactor is connected with the import of absorbent charcoal adsorber with the first cooling, and the first cooling is connected with the import of the first dilute sulfuric acid surge tank with the outlet of absorbent charcoal adsorber；Second outlet of extraction reactor is connected with the import of back extraction reactor, and the first outlet of back extraction reactor is connected with the import of absorbent charcoal adsorber with the second cooling, and the second cooling is connected with the import of nitrobased NPK storage tank with the outlet of absorbent charcoal adsorber；Second outlet of back extraction reactor is connected with the second import of extraction reactor.
Preferably, described reduction apparatus includes preheating device, hydrogenation reactor, cooling device, gas-liquid separator separates, amino T acid storage tank, filter, the material inlet of preheating device is connected with the outlet of nitrobased NPK storage tank, the outlet of preheating device is connected with the first import of hydrogenation reactor, the outlet of hydrogenation reactor is connected with the import of cooling device, the material outlet of cooling device is connected with the import of gas-liquid separator separates, the liquid outlet of gas-liquid separator separates is connected with the import of amino T acid storage tank, the gas vent of gas-liquid separator separates is connected with the import of filter, the outlet of filter is connected with the second import of hydrogenation reactor.
Preferably, described enrichment facility includes the second preheating device, 5 effect adverse current enrichment facilities, dense T acid buffering tank, 2 effect adverse current enrichment facility, dope alkali surge tanks, first import of the second preheating device is connected with the delivery port of cooling device, second import of the second preheating device is connected with the outlet of amino T acid storage tank, the outlet of the second preheating device is connected with the import of 5 effect adverse current enrichment facilities, and the outlet of 5 effect adverse current enrichment facilities is connected with the import of dense T acid buffering tank；The 2 effect adverse current outlets of enrichment facility are connected with the import of dope alkali surge tank.
Preferably, described air mix facilities includes heat exchanger, alkali-melting vessel, preheater, the 3rd pump, dilution still, condensate recycling device, stripper, methanol recovery device and alkali fusion thing surge tank, the import of described heat exchanger is connected with the outlet of dope alkali surge tank, the outlet of heat exchanger is connected with the first import of alkali-melting vessel, and the dense outlet of T acid buffering tank is connected with the second entrance of preheater；The outlet of preheater is connected with the second import of alkali-melting vessel by the 3rd pump, the outlet of alkali-melting vessel is connected with the import of dilution still, the methanol outlet of dilution still is connected with the import of condensate recycling device, and the outlet of condensate recycling device is connected with the first import of methanol recovery device；The alkali fusion thing outlet of dilution still is connected with the entrance of stripper, and the methanol outlet of stripper is connected with the second import of methanol recovery device, and the outlet of methanol recovery device is connected with preheater the first import；The alkali fusion thing outlet of stripper is connected with the import of alkali fusion thing surge tank.
Preferably, described isolation and filter include acid preparing device, the second dilute sulfuric acid surge tank, separation kettle, the second cooling device, cooling reactor, filter, sulfur dioxide recovery device, wash water tank, wastewater treatment equipment；The import of acid preparing device is connected with the outlet of the first dilute sulfuric acid surge tank, the outlet of acid preparing device is connected with the import of the second dilute sulfuric acid surge tank, the outlet of the second dilute sulfuric acid surge tank and the first import of separation kettle connect, second import of separation kettle and the outlet of alkali fusion thing surge tank connect, the sulfur dioxide outlet of separation kettle and the import of the second cooling device connect, the outlet of the second cooling device and the import of sulfur dioxide recovery device connect, the material outlet of separation kettle is connected with the import of cooling reactor, the outlet of cooling reactor and the entrance of filter connect, first outlet of filter and the entrance of wash water tank connect, the outlet of wash water tank is connected with the triple feed inlet of separation kettle, second outlet of filter and the import of wastewater treatment equipment connect.
As preference, the described H-acid preparation facilities with energy-saving effect, also including drying device, the import of drying device and the 3rd outlet of filter connect.
Beneficial effect: compared with prior art, the embodiment of the present invention has the advantages that above-described embodiment prepares H-acid through extraction equipment, reduction apparatus, enrichment facility, air mix facilities, isolation and filter.Utilize this device to produce H-acid and there is continuity, substantially increase production efficiency.Simultaneously in preparation process, part material is reclaimed, recycling, greatly reduce financial cost.
Accompanying drawing explanation
Fig. 1 is a kind of structured flowchart of the embodiment of the present invention；
Fig. 2 is the another kind of structured flowchart of the embodiment of the present invention；
Fig. 3 is the structured flowchart after the embodiment of the present invention and xanthator, nitrification installation 2, denitrification apparatus assembling.
nullFigure has: xanthator 1、Nitrification installation 2、Denitrification apparatus 3、Extraction equipment 4、Reduction apparatus 5、Enrichment facility 6、Air mix facilities 7、Isolation and filter 8、Drying device 9、Sulphonation kettle 101、Surge tank 102、Indexing sulfonation tower 103、Sulfonation reactor 104、Three sulfonation towers 105、Sulfonated bodies surge tank 106、One-level nitrator 201、Two grades of nitrating pots 202、Itrated compound surge tank 203、First pump 301、Benitration reactor 302、Denitration thing surge tank 303、Second pump 401、Extraction reactor 402、First cooling and absorbent charcoal adsorber 403、First dilute sulfuric acid surge tank 404、Back extraction reactor 405、Second cooling and absorbent charcoal adsorber 406、Nitrobased NPK storage tank 407、Preheating device 501、Hydrogenation reactor 502、Cooling device 503、Gas-liquid separator separates 504、Amino T acid storage tank 505、Filter 506、Second preheating device 601、5 effect adverse current enrichment facilities 602、Dense T acid buffering tank 603、2 effect adverse current enrichment facilities 604、Dope alkali surge tank 605、Heat exchanger 701、Alkali-melting vessel 702、Preheater 703、3rd pump 704、Dilution still 705、Condensate recycling device 706、Stripper 707、Methanol recovery device 708、Alkali fusion thing surge tank 709、Acid preparing device 801、Second dilute sulfuric acid surge tank 802、Separation kettle 803、Second cooling device 804、Cooling reactor 805、Filter 806、Sulfur dioxide recovery device 807、Wash water tank 808、Wastewater treatment equipment 809.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is described in detail.
As it is shown in figure 1, a kind of H-acid preparation facilities with energy-saving effect of the embodiment of the present invention, this device includes extraction equipment 4, reduction apparatus 5, enrichment facility 6, air mix facilities 7, isolation and filter 8.The outlet of xanthator 1 is connected with the import of nitrification installation 2, the outlet of nitrification installation 2 is connected with the import of denitrification apparatus 3, the outlet of denitrification apparatus 3 is connected with the import of extraction equipment 4, first outlet of extraction equipment 4 is connected with the import of reduction apparatus 5, the outlet of reduction apparatus 5 is connected with the import of enrichment facility 6, the outlet of enrichment facility 6 is connected with the import of air mix facilities 7, the outlet of air mix facilities 7 is connected with the first import of isolation and filter 8, and the second outlet of isolation and the second import of filter 8 and extraction equipment 4 connects.
Above-described embodiment prepares H-acid through xanthator 1, nitrification installation 2, denitrification apparatus 3, extraction equipment 4, reduction apparatus 5, enrichment facility 6, air mix facilities 7, isolation and filter 8, drying device 9.Utilize this device to produce H-acid and there is continuity.Use closed reaction simultaneously, reduce waste gas and the uncontrollable discharge of waste liquid.
The present embodiment uses solvent extraction technology to replace crude salt analysis technique, has not only saved a large amount of neutralization ammoniacal liquor, and has decreased the generation of T-acid isolation waste water.Meanwhile, the second outlet of isolation and the second import of filter 8 and extraction equipment 4 connects, and is used in isolation and filter 8 by the dilute sulfuric acid produced, decreases the sulfuric acid usage amount of H-acid isolation in extraction equipment 4.Only this step can make yield improve about 10%, saves substantial amounts of resource consumption simultaneously.The present embodiment uses 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.
In above-described embodiment, extraction equipment 4 carries out extraction process to denitration thing, obtains dilute sulfuric acid and extraction mixture, and extraction mixture is carried out back extraction, obtain nitrobased NPK solution.Preferably, cool down and absorbent charcoal adsorber 406, nitrobased NPK storage tank 407 as it is shown in figure 1, described extraction equipment 4 includes that the second pump 401, extraction reactor 402, first cool down with absorbent charcoal adsorber the 403, first dilute sulfuric acid surge tank 404, back extraction reactor 405, second；The import of the second pump 401 is connected with the outlet of denitration thing surge tank 303, the outlet of the second pump 401 is connected with the first import of extraction reactor 402, first outlet of extraction reactor 402 is connected with the import of absorbent charcoal adsorber 403 with the first cooling, and the first cooling is connected with the import of the first dilute sulfuric acid surge tank 404 with the outlet of absorbent charcoal adsorber 403；Second outlet of extraction reactor 402 is connected with the import of back extraction reactor 405, first outlet of back extraction reactor 405 is connected with the import of absorbent charcoal adsorber 406 with the second cooling, and the second cooling is connected with the import of nitrobased NPK storage tank 407 with the outlet of absorbent charcoal adsorber 406；Second outlet of back extraction reactor 405 is connected with the second import of extraction reactor 402.
When extraction equipment 4 works, denitration thing, extractant and the water generated by denitrification apparatus 3 continues through the second pump 401 and sends into extraction reactor 402, after four-stage counter-current extractive reaction, is extracted mixture and dilute sulfuric acid.By dilute sulfuric acid after the first cooling processes with absorbent charcoal adsorber 403, it is stored in the first dilute sulfuric acid surge tank 404.Extraction mixture liquid caustic soda is carried out back extraction in back extraction reactor 405, it is extracted agent and nitrobased NPK solution, extractant is returned in extraction reactor 402 by the second outlet of back extraction reactor 405, carry out extractive reaction, and by nitrobased NPK solution after the second cooling processes with absorbent charcoal adsorber 406, deliver in nitrobased NPK storage tank 407.
TEHA selected by extractant, and molecular formula formula is: C24H51N.Extraction process and back extraction process chemical equation are expressed as follows:
In back extraction reactor 405, after carrying out back extraction process, the extractant generated is returned in extraction reactor 402, carries out extractive reaction.The extractant quantity needed during being thus greatly saved extractive reaction so that extractant, during producing H-acid continuously, can be reused, reduce cost.
In above-described embodiment, reduction apparatus 5, for nitrobased NPK solution is carried out reduction treatment, obtains amino T acid solution.As it is shown in figure 1, described reduction apparatus 5 includes preheating device 501, hydrogenation reactor 502, cooling device 503, gas-liquid separator separates 504, amino T acid storage tank 505, filter 506.The material inlet of preheating device 501 is connected with the outlet of nitrobased NPK storage tank 407, the outlet of preheating device 501 is connected with the first import of hydrogenation reactor 502, the outlet of hydrogenation reactor 502 is connected with the import of cooling device 503, the material outlet of cooling device 503 is connected with the import of gas-liquid separator separates 504, the liquid outlet of gas-liquid separator separates 504 is connected with the import of amino T acid storage tank 505, the gas vent of gas-liquid separator separates 504 is connected with the import of filter 506, and the outlet of filter 506 is connected with the second import of hydrogenation reactor 502.
When reduction apparatus 5 works, by catalyst, hydrogen, nitrobased NPK solution after preheating device 501 preheats, deliver in hydrogenation reactor 502,170 DEG C, carry out hydrogenation reduction under 20MPa.After reaction terminates, with water, material is cooled to 90 DEG C, obtains reactant mixture.In cooling device 503, the hot water produced after cooling is amino T acid preheating in subsequent step.Reactant mixture is separated through gas-liquid separator 504, and after release, obtains amino T acid solution and catalyst.Amino T acid solution is delivered in amino T acid storage tank 505.Utilize filter 506 to reclaim catalyst, and the catalyst of recovery is recycled and reused in hydrogenation reactor 502.
As preferably, catalyst is Raney's nickel.The chemical equation occurred in reduction apparatus 5 is expressed as follows:
In reduction apparatus 5, after material being cooled to 90 DEG C with water, water becomes hot water, may be used for amino T acid preheating 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, during producing H-acid continuously, makes full use of existing material, and reused, advantageously reduce cost.
In above-described embodiment, enrichment facility 6 is used for amino T acid solution and liquid caustic soda are carried out concentration respectively, the amino T acid solution after being concentrated and liquid caustic soda.As it is shown in figure 1, described enrichment facility 6 includes the second preheating device 601,5 effect adverse current enrichment facility 602, dense T acid buffering tank 603,2 effect adverse current enrichment facility 604, dope alkali surge tank 605.First import of the second preheating device 601 is connected with the delivery port of cooling device 503, second import of the second preheating device 601 is connected with the outlet of amino T acid storage tank 505, the outlet of the second preheating device 601 is connected with the import of 5 effect adverse current enrichment facilities 602, and the outlet of 5 effect adverse current enrichment facilities 602 is connected with the import of dense T acid buffering tank 603；The 2 effect adverse current outlets of enrichment facility 604 are connected with the import of dope alkali surge tank 605.
When enrichment facility 6 works, utilize the hot water that cooling device 503 delivery port flows out, amino T acid solution is preheated, be concentrated into setting concentration through 5 effect adverse current enrichment facilities 602, be then sent in dense T acid buffering tank 603.Liquid caustic soda is concentrated into, through 2 effect adverse current enrichment facilities 604, the liquid caustic soda that mass concentration is 72%, is then sent in dope alkali surge tank 605.
In above-described embodiment, air mix facilities 7 carries out alkali fusion process to the amino T acid solution after concentrating and liquid caustic soda, and is diluted processing, the alkali fusion thing after being diluted.As it is shown in figure 1, described air mix facilities 7 includes heat exchanger 701, alkali-melting vessel 702, preheater the 703, the 3rd pump 704, dilution still 705, condensate recycling device 706, stripper 707, methanol recovery device 708 and alkali fusion thing surge tank 709.The import of described heat exchanger 701 is connected with the outlet of dope alkali surge tank 605, and the outlet of heat exchanger 701 is connected with the first import of alkali-melting vessel 702, and the dense outlet of T acid buffering tank 603 is connected with the second entrance of preheater 703；The outlet of preheater 703 is connected with the second import of alkali-melting vessel 702 by the 3rd pump 704, the outlet of alkali-melting vessel 702 is connected with the import of dilution still 705, the methanol outlet of dilution still 705 is connected with the import of condensate recycling device 706, and the outlet of condensate recycling device 706 is connected with the first import of methanol recovery device 708；The alkali fusion thing outlet of dilution still 705 is connected with the entrance of stripper 707, and the methanol outlet of stripper 707 is connected with the second import of methanol recovery device 708, and the outlet of methanol recovery device 708 is connected with preheater 703 first import；The alkali fusion thing outlet of stripper 707 is connected with the import of alkali fusion thing surge tank 709.
When air mix facilities 7 works, liquid caustic soda after concentrating is preheated to 180 DEG C through heat exchanger 701, it is then fed in alkali-melting vessel 702, after subsequently the amino T acid solution after methyl alcohol and concentration being preheated by preheater 703 respectively, pump into alkali-melting vessel 702 by the 3rd pump 704, liquid caustic soda, methyl alcohol and amino T acid solution 200 DEG C, react under 2.8MPa, after reaction terminates, by material press-in dilution still 705 is diluted with water, obtain the alkali fusion thing after dilute methanol and dilution.Reclaiming, by condensate recycling device 706 condensation, the dilute methanol steamed, the alkali fusion thing after dilution reclaims residual methanol through stripper 707.Dilute methanol is delivered in methanol recovery device 708, and methanol recovery device 708 is connected with preheater 703 first import, for the methyl alcohol of recovery being used for alkali fusion reaction next time.Alkali fusion thing after dilution is sent in alkali fusion thing surge tank 709.
The chemical equation occurred in air mix facilities 7 is expressed as follows:
In above-described embodiment, isolation and filter 8, to the alkali fusion thing after dilution, carry out isolating and filtration treatment, obtain H-acidleach cake.As it is shown in figure 1, described isolation and filter 8 include acid preparing device the 801, second dilute sulfuric acid surge tank 802, separation kettle the 803, second cooling device 804, cooling reactor 805, filter 806, sulfur dioxide recovery device 807, wash water tank 808, wastewater treatment equipment 809.nullThe import of acid preparing device 801 is connected with the outlet of the first dilute sulfuric acid surge tank 404，The outlet of acid preparing device 801 is connected with the import of the second dilute sulfuric acid surge tank 802，The outlet of the second dilute sulfuric acid surge tank 802 and the first import of separation kettle 803 connect，Second import of separation kettle 803 and the outlet of alkali fusion thing surge tank 709 connect，The sulfur dioxide outlet of separation kettle 803 and the import of the second cooling device 804 connect，The outlet of the second cooling device 804 and the import of sulfur dioxide recovery device 807 connect，The material outlet of separation kettle 803 is connected with the import of cooling reactor 805，The outlet of cooling reactor 805 and the entrance of filter 806 connect，First outlet of filter 806 and the entrance of wash water tank 808 connect，The outlet of wash water tank 808 is connected with the triple feed inlet of separation kettle 803，Second outlet of filter 806 and the import of wastewater treatment equipment 809 connect，3rd outlet of filter 806 and the import of drying device 9 connect.
When isolation and filter 8 work, first complex acid process is carried out: by the dilute sulfuric acid in the first dilute sulfuric acid surge tank 404, mix in acid preparing device 801 with the sulfuric 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 802.Then isolation process is carried out: by the dilute sulfuric acid in the alkali fusion thing in alkali fusion thing surge tank 709, H-acid washing water and the second dilute sulfuric acid surge tank 802, deliver to separation kettle 803 is carried out isolation process, the sulfur dioxide produced, after the second cooling device 804 cooling, is reclaimed by sulfur dioxide recovery device 807 liquefaction.Finally carry out cooling down and filtration treatment: by the material after isolation processes, cooled still 805 continuous coo1ing, to 50 DEG C, filters with filter 806, washes, and obtains H-acidleach cake, wash water and mother liquor, wash water is stored in wash water tank 808, processes for isolation next time；Mother liquor is delivered in wastewater treatment equipment 809.
The chemical equation occurred in isolation and filter 8 is expressed as follows:
H2SO4+2NaOH→Na2SO4+2H2O
H2SO4+Na2SO3→Na2SO4+SO2+H2O
As in figure 2 it is shown, described device also includes drying device 9.From the H-acidleach cake entrance drying device 9 that the 3rd outlet of filter 806 leaches, it is dried process, prepares H-acid.H-acidleach cake can be dried tail gas and enter air by heated-air drying in spin flash dryer after cyclonic separation, bag-type dust；The H-acid finished product obtained, is then fed into subsequent packages operation.
When denitration thing is extracted by extraction equipment 4, denitration thing is made up through xanthator 1, nitrification installation 2 and denitrification apparatus 3 of liquid naphthalene.
Xanthator 1 is used for generating sulfonated bodies.Preferably, as it is shown on figure 3, described xanthator 1 includes sulphonation kettle 101, surge tank 102, indexing sulfonation tower 103,104, three sulfonation towers 105 of sulfonation reactor and sulfonated bodies surge tank 106.The outlet of sulphonation kettle 101 is connected with the import of surge tank 102, the outlet of surge tank 102 is connected with the import of indexing sulfonation tower 103, the indexing outlet of sulfonation tower 103 is connected with the import of sulfonation reactor 104, the outlet of sulfonation reactor 104 is connected with the import of three sulfonation towers 105, and the outlet of three sulfonation towers 105 is connected with the import of sulfonated bodies surge tank 106.
When above-mentioned xanthator 1 works, liquid naphthalene and the sulfuric acid solution that mass concentration is 100% being continuously added in sulphonation kettle 101, the temperature in sulphonation kettle 101 is 90 DEG C, carries out sulfonation for the first time.Being continuously introduced into after the buffered tank of product after first time sulfonation 102 in indexing sulfonation tower 103, the temperature in indexing sulfonation tower 103 is 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 104, in sulfonation reactor 104, temperature is 65 DEG C, carries out second time sulfonation.Three sulfonation towers 105 delivered to by material and oleum after second time sulfonation being completed, and the temperature in three sulfonation towers 105 is 150 DEG C, carry out third time sulfonation, generate sulfonated bodies, and sulfonated bodies is sent into storage in sulfonated bodies surge tank 106.The chemical equation occurred in xanthator 1 is as follows:
Nitrification installation 2 is used for generating itrated compound.Preferably, as shown in Figure 3, described nitrification installation 2 includes 201, two grades of nitrating pots 202 of one-level nitrator and itrated compound surge tank 203, the import of one-level nitrator 201 is connected with the outlet of sulfonated bodies surge tank 106, the outlet of one-level nitrator 201 is connected with the import of two grades of nitrating pots 202, and the outlet of two grades of nitrating pots 202 is connected with the entrance of itrated compound surge tank 203.
During work, sulfonated bodies and the nitric acid that mass concentration is 68% of storage in sulfonated bodies surge tank 106 are continuously pumped in one-level nitrator 201, and in 40 DEG C of nitrifications under cooling water cooling, then overflow is in two grades of nitrating pots 202, complete nitration reaction, the itrated compound generated is sent in itrated compound surge tank 203 store after reaction.
The chemical equation occurred in nitrification installation 2 is as follows:
Denitrification apparatus 3 is used for generating denitration thing.Preferably, as shown in Figure 3, denitrification apparatus 3 includes the first pump 301, Benitration reactor 302 and denitration thing surge tank 303, the outlet of the first pump 301 is connected with the first import of Benitration reactor 302, second import of Benitration reactor 302 is connected with the outlet of itrated compound surge tank 203, and the outlet of Benitration reactor 302 is connected with the import of denitration thing surge tank 303.
During work, squeezing in Benitration reactor 302 with pump 301 by water, simultaneously by the itrated compound feeding Benitration reactor 302 of storage in itrated compound surge tank 203, homogeneous mixture of material, generation denitration thing, after cooling, in denitration thing sends into denitration thing surge tank 303.The nitrogen oxide gas produced during denitration reaction, condensed rear alkali lye, such as NaOH absorb, enter air after reaching standard.
The general principle of the present invention, principal character and advantage have more than been shown and described.Those skilled in the art it should be recognized that; the present invention is not limited by above-mentioned specific embodiment; description in above-mentioned specific embodiment and specification is intended merely to further illustrate the principle of the present 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 scope of the claimed invention.The scope of protection of present invention is defined by claims and equivalent thereof.
Claims (7)
1. a H-acid preparation facilities with energy-saving effect, it is characterized in that, this device includes extraction equipment (4), reduction apparatus (5), enrichment facility (6), air mix facilities (7), isolation and filter (8), first outlet of extraction equipment (4) is connected with the import of reduction apparatus (5), the outlet of reduction apparatus (5) is connected with the import of enrichment facility (6), the outlet of enrichment facility (6) is connected with the import of air mix facilities (7), the outlet of air mix facilities (7) is connected with the first import of isolation and filter (8), second outlet of isolation and the second import of filter (8) and extraction equipment (4) connects.
2. according to the H-acid preparation facilities with energy-saving effect described in claim 1, it is characterized in that, described extraction equipment (4) includes the second pump (401), extraction reactor (402), the first cooling and absorbent charcoal adsorber (403), the first dilute sulfuric acid surge tank (404), back extraction reactor (405), the second cooling and absorbent charcoal adsorber (406), nitrobased NPK storage tank (407)；The import of the second pump (401) is connected with the outlet of denitration thing surge tank (303), the outlet of the second pump (401) is connected with the first import of extraction reactor (402), first outlet of extraction reactor (402) is connected with the import of absorbent charcoal adsorber (403) with the first cooling, and the first cooling is connected with the import of the first dilute sulfuric acid surge tank (404) with the outlet of absorbent charcoal adsorber (403)；Second outlet of extraction reactor (402) is connected with the import of back extraction reactor (405), first outlet of back extraction reactor (405) is connected with the import of absorbent charcoal adsorber (406) with the second cooling, and the second cooling is connected with the import of nitrobased NPK storage tank (407) with the outlet of absorbent charcoal adsorber (406)；Second outlet of back extraction reactor (405) is connected with the second import of extraction reactor (402).
null3. according to the H-acid preparation facilities with energy-saving effect described in claim 1，It is characterized in that，Described reduction apparatus (5) includes preheating device (501)、Hydrogenation reactor (502)、Cooling device (503)、Gas-liquid separator separates (504)、Amino T acid storage tank (505)、Filter (506)，The material inlet of preheating device (501) is connected with the outlet of nitrobased NPK storage tank (407)，The outlet of preheating device (501) is connected with the first import of hydrogenation reactor (502)，The outlet of hydrogenation reactor (502) is connected with the import of cooling device (503)，The material outlet of cooling device (503) is connected with the import of gas-liquid separator separates (504)，The liquid outlet of gas-liquid separator separates (504) is connected with the import of amino T acid storage tank (505)，The gas vent of gas-liquid separator separates (504) is connected with the import of filter (506)，The outlet of filter (506) is connected with the second import of hydrogenation reactor (502).
4. according to the H-acid preparation facilities with energy-saving effect described in claim 1, it is characterized in that, described enrichment facility (6) includes the second preheating device (601), 5 effects adverse current enrichment facility (602), dense T acid buffering tank (603), 2 effects adverse current enrichment facility (604), dope alkali surge tank (605)
First import of the second preheating device (601) is connected with the delivery port of cooling device (503), second import of the second preheating device (601) is connected with the outlet of amino T acid storage tank (505), the outlet of the second preheating device (601) is connected with the import of 5 effects adverse current enrichment facility (602), and the outlet of 5 effects adverse current enrichment facility (602) is connected with the import of dense T acid buffering tank (603)；The outlet of 2 effects adverse current enrichment facility (604) is connected with the import of dope alkali surge tank (605).
5. according to the H-acid preparation facilities with energy-saving effect described in claim 1, it is characterized in that, described air mix facilities (7) includes heat exchanger (701), alkali-melting vessel (702), preheater (703), 3rd pump (704), dilution still (705), condensate recycling device (706), stripper (707), methanol recovery device (708) and alkali fusion thing surge tank (709), the import of described heat exchanger (701) is connected with the outlet of dope alkali surge tank (605), the outlet of heat exchanger (701) is connected with the first import of alkali-melting vessel (702), the outlet of dense T acid buffering tank (603) is connected with the second entrance of preheater (703)；The outlet of preheater (703) is connected with the second import of alkali-melting vessel (702) by the 3rd pump (704), the outlet of alkali-melting vessel (702) is connected with the import of dilution still (705), the methanol outlet of dilution still (705) is connected with the import of condensate recycling device (706), and the outlet of condensate recycling device (706) is connected with the first import of methanol recovery device (708)；The alkali fusion thing outlet of dilution still (705) is connected with the entrance of stripper (707), the methanol outlet of stripper (707) is connected with the second import of methanol recovery device (708), and the outlet of methanol recovery device (708) is connected with preheater (703) first import；The alkali fusion thing outlet of stripper (707) is connected with the import of alkali fusion thing surge tank (709).
6. according to the H-acid preparation facilities with energy-saving effect described in claim 1, it is characterized in that, described isolation and filter (8) include acid preparing device (801), the second dilute sulfuric acid surge tank (802), separation kettle (803), the second cooling device (804), cooling reactor (805), filter (806), sulfur dioxide recovery device (807), wash water tank (808), wastewater treatment equipment (809)；
nullThe import of acid preparing device (801) is connected with the outlet of the first dilute sulfuric acid surge tank (404)，The outlet of acid preparing device (801) is connected with the import of the second dilute sulfuric acid surge tank (802)，The outlet of the second dilute sulfuric acid surge tank (802) and the first import of separation kettle (803) connect，Second import of separation kettle (803) and the outlet of alkali fusion thing surge tank (709) connect，The sulfur dioxide outlet of separation kettle (803) and the import of the second cooling device (804) connect，The outlet of the second cooling device (804) and the import of sulfur dioxide recovery device (807) connect，The material outlet of separation kettle (803) is connected with the import of cooling reactor (805)，The outlet of cooling reactor (805) and the entrance of filter (806) connect，First outlet of filter (806) and the entrance of wash water tank (808) connect，The outlet of wash water tank (808) is connected with the triple feed inlet of separation kettle (803)，Second outlet of filter (806) and the import of wastewater treatment equipment (809) connect.
7., according to the H-acid preparation facilities with energy-saving effect described in claim 1, it is characterised in that also include drying device (9), the import of drying device (9) and the 3rd outlet of filter (806) connect.
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| CN108191717A (en) * | 2017-11-27 | 2018-06-22 | 江苏力禾颜料有限公司 | H acid isolates preparation process |
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