CN105384713A - Furfural refining deacidification method and system capable of effectively reducing furfural acid value and meeting drainage standard - Google Patents
Furfural refining deacidification method and system capable of effectively reducing furfural acid value and meeting drainage standard Download PDFInfo
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- CN105384713A CN105384713A CN201510658290.3A CN201510658290A CN105384713A CN 105384713 A CN105384713 A CN 105384713A CN 201510658290 A CN201510658290 A CN 201510658290A CN 105384713 A CN105384713 A CN 105384713A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
Abstract
The present invention discloses a furfural refining deacidification method capable of effectively reducing a furfural acid value and meeting a drainage standard. In a furfural refining process, after being diluted with demineralized water, a deacidification agent is injected into a furfural refining aqueous solution system and is subjected to a furfural refining treatment. The furfural refining deacidification method is characterized in that the deacidification agent comprises the following components in percentage by mass: 30%-55% of organic amine, 20%-40% of a demulsifying agent and 10%-40% of a mixed solvent; and the demulsifying agent is one of or a combination of two of a nonionic polyacrylamide demulsifier and a small molecule branched structured polymer. The present invention also discloses a furfural apparatus water system which implements the method. According to the method and system disclosed by the present invention, furfural acid, naphthenic acid and other acidic substances in the furfural can be effectively neutralised so as to reduce the furfural acid value, furthermore, the demulsifier in the deacidification agent can effectively prevent the furfural from being emulsified with water, the separation of the furfural and the water is facilitated, and the COD value of the water can be greatly reduced.
Description
Technical field
The present invention relates to a kind of furfural treatment acid stripping method, particularly relate to and a kind ofly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard.The invention still further relates to the system implementing the method.
Background technology
Furfural extraction unit is using furfural as extraction solvent, according to the selectivity of furfural, removes the undesirable components in lubricant base, reaches refining object.Processing sulfur-bearing raw material can make furfural extraction unit seriously corroded, and especially the corrosion of furfural aqueous solution recovery system is particularly serious.The oxidation stability of furfural is poor, under the effect of air, water, sunlight, be very easily oxidized to furfural acid, has stronger corrodibility, and can be polymerized spanning tree smectic oxide compound further, last condensation coking.Aborning, due to furfural recycle, furfural is constantly oxidized, and furfural, furfural acid, water become ternary azeotrope, and the system furfural acid of making cannot be separated, and constantly accumulates, and causes circulation furfural acidity high.In addition, acidic substance (naphthenic acid is main) in decompression side line distillate can by furfural solvent extracting, but the boiling point naphthenic acid close with furfural boiling point in solvent recuperation with furfural circulation, have accumulated naphthenic acid, facilitate circulation furfural acidity to raise, refining effect is poor.Stoping furfural oxidation, going bad is improve the basic effective way of furfural extraction unit.Although take some physical protection measures, as done degassing tower degassing operation well, furfural storage tank adds oil sealing, control furnace outlet temperature, adopt stainless steel to improve equipment anticorrosion ability etc., play corrosion inhibition to a certain extent, but furfural can not be stoped to be oxidized, in and furfural oxide compound.
Chemical Preservation technology is utilized to solve furfural aqueous solution recovery system caustic solution, as periodical " Maoming petrochemical complex " 2005.1(20 page) " utilizing DY-06 de-acidying agent to reduce heavy furfural refining oil neutralization value " introduce: after the outlet valve of furfural treatment aqueous solution system, add a kind of organic macromolecule ammonia, by acid-base neutralisation reaction reduction system furfural acidity, neutralized reaction product enters aqueous solution recovery tower with the aqueous solution, and discharges with tower draining.But in practice, there are the following problems for the method: (1) injects this de-acidying agent, organic macromolecule ammonia and furfural acid generate furfural acid amine salt, furfural acid amine salt can make the emulsifying property of water increase, aldehyde and aquatic products lactogenesis, and aldehyde water stratification is unintelligible, general demulsifying agent all cannot make it obvious layering, emulsion separates difficulty, cause dehydration tower draining COD value large, device efflux wastewater is not up to standard.(2) corrosion and the coking of furfural extraction unit pumped vacuum systems water-sealed tank cannot be alleviated.Because furfural self-polymerization generates burnt class macromole, the big and small burnt dirt of high more than half meter is often full of in vacuum water sealed cans, the water of top is taken out pipeline and water and is taken out nozzle and easily blocked by burnt grain in tank, and general one and a half months is removed water and taken out pipeline and nozzle decoking, and labour intensity is large.The very large adhesivity jelly that has that device can generate because of furfural coking is attached to vacuum water sealed cans and water takes out pipeline inwall, be piled into very thick very hard Jiao dirt, if cannot remove during maintenance, just have to have changed new corrosion resistant stainless steel water sealed cans and water takes out pipeline, increase production cost.
As shown in Figure 1, furfural device aqueous solution system, form primarily of water-soluble flow container 405, drying tower 406, dehydration tower 407 and vacuum water sealed cans 410, water-soluble flow container 405 is connected with drying tower 406 and dehydration tower 407 respectively, stripping tower top 402 and 405 is out containing the solvent of large water gaging, enter in aqueous solution tank 405 after watercooler 4 cools and carry out layering, upper water solution water is pumped in dehydration tower 407 dewaters, and the furfural just evaporated returns in water-soluble flow container 405 after water cooler cooling in point flow container 403/2.Lower floor's furfural is pumped to drying tower 406 through furfural and carries out drying, to be out recycled to water-soluble flow container 405 after water cooler cooling to be separated by the water that evaporates from tower top.Vacuum water sealed cans 410 are connected with vacuum tank 403/1.De-acidying agent tank 411 is connected with the pipeline between water-soluble flow container 405 with the outlet valve of vacuum tank 403/1 through de-acidying agent pump 412 and pipeline, injects de-acidying agent in this place.
Summary of the invention
An object of the present invention is to provide a kind of can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard.
Two of object of the present invention is to provide a kind of furfural treatment aqueous solution system implementing above-mentioned method.
First object of the present invention is achieved through the following technical solutions: a kind ofly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, in furfural treatment technique, de-acidying agent is with after softening water dilution, inject furfural treatment aqueous solution system, participate in furfural treatment process, wherein said de-acidying agent comprises the component of following mass percent:
Organic amine 30% ~ 55%
Demulsifying agent 20% ~ 40%
Complex solvent 10% ~ 40%;
Described demulsifying agent is one or both combination in non-ionic polyacrylamide type emulsion splitter and small molecules branched structure polymkeric substance.
In the present invention, utilize the organic amine in de-acidying agent and furfural acid to react, generate furfural acid amine salt.Although furfural acid amine salt can make the emulsifying property of water increase, make water and furfural emulsification, but because demulsifying agent adopts non-ionic polyacrylamide type emulsion splitter and/or small molecules branched structure polymkeric substance, reduce the emulsifying property of water, make the settlement separate smooth and easy of furfural and water, layering is obvious, contributes to the separation of furfural water system solution, reduce the COD value of the aqueous solution, make draining reach standard of drainage.
Organic amine of the present invention is one or both the combination in diethanolamine, trolamine, Main Function be in and furfural acid and naphthenic acid.
Demulsifying agent of the present invention is one or both combinations in water-soluble demulsifier JH-3 and JH-5, and JH-3 type emulsion splitter is non-ionic polyacrylamide type emulsion splitter, and surface wettability is strong, the water purification that tool is good; JH-5 type emulsion splitter is small molecules branched structure polymkeric substance, and dispersed and interface is substituting comparatively strong, can make aldehyde water termination short texture, reduce interface film strength, have breaking emulsion and dewatering function.
Also comprise inhibiter in the present invention, its mass percentage content in de-acidying agent is 1 ~ 5%.Described inhibiter is vulkacit H, can reduce the corrosion of acidic substance to device metal surface.
Complex solvent of the present invention is water.
The preparation method of de-acidying agent of the present invention is:
(1) organic amine, demulsifying agent and complex solvent is taken in proportion;
(2) in heating stirrer, first add organic amine, complex solvent, at 40 ~ 60 DEG C, stir 20min, make it fully dissolve;
(3) add described inhibiter and demulsifying agent again, keep stirring 30 ~ 40min at 50 ~ 70 DEG C, obtain de-acidying agent finished product.
De-acidying agent of the present invention needs to be diluted to through softening water the aqueous solution that concentration is 3% ~ 10% before use.
De-acidying agent of the present invention can only inject in water-soluble flow container.Also further, de-acidying agent can be injected respectively in vacuum water sealed cans and water-soluble flow container, corrosion and the coking of furfural extraction unit pumped vacuum systems water-sealed tank can be alleviated like this while depickling, prevent water at the bottom of tank from taking out line and blocked by Jiao.
Further, described de-acidying agent from de-acidying agent tank out after be divided into two sections through pipeline and inject furfural treatment aqueous solution systems, one section is injected vacuum water sealed cans, and another section is injected into water-soluble flow container.When adopting in this way, de-acidying agent tank is arranged at the position higher than water-soluble flow container and vacuum water sealed cans, itself and vacuum water sealed cans and water-soluble flow container position height difference are at least 3 meters, liquid self-pressure can be utilized like this in vacuum water sealed cans and water-soluble flow container to inject de-acidying agent, de-acidying agent pump need not be used, save energy.
In the present invention, the de-acidying agent concentration injected in furfural device is 30 ~ 40ppm.In depickling treating processes, the temperature of water-soluble flow container is kept to be 40 ~ 55 DEG C.
Second object of the present invention is achieved through the following technical solutions: a kind of furfural treatment aqueous solution system implementing above-mentioned method, comprise de-acidying agent tank, vacuum tank, water-soluble flow container, drying tower, dehydration tower and vacuum water sealed cans are formed, water-soluble flow container is connected with drying tower and dehydration tower respectively, the top gas outlet of drying tower and dehydration tower is connected to water-soluble flow container through water cooler and a point flow container respectively, vacuum water sealed cans are connected with vacuum tank, it is characterized in that, described de-acidying agent tank is arranged at the position higher than water-soluble flow container and vacuum water sealed cans, its liquid outlet divides two pipelines to be connected with water-soluble flow container and vacuum water sealed cans respectively, form two-way de-acidying agent and inject route.
Described de-acidying agent tank and vacuum water sealed cans and water-soluble flow container position height difference are at least 3 meters.
the present invention compared with prior art has following technique effect:
To more, the good DY-06 de-acidying agent of effect be selected in de-acidying agent of the present invention and internal lube oil furfural extraction unit to make reference, evaluation result be as follows:
1. by de-acidying agent of the present invention and DY-06 de-acidying agent distilled water diluting to 1%, get the circulation furfural that 200ml furfural extraction unit is adopted back, add diluted de-acidying agent 0.6ml, add 80ml distilled water again, separate aqueous layer after abundant stirring, get furfural and analyze acid number, test-results is in table 1.
As shown in Table 1, de-acidying agent of the present invention can better reduce the acidity of circulation furfural relative to existing de-acidying agent.2. de-acidying agent physical and chemical index of the present invention is in table 2.
3. for investigating demulsifying agent add-on to the impact of circulation furfural acidity, take from five kinds of different composition de-acidying agent distilled water dilutings to 1% of table 3, get the circulation furfural (acidity 23.83mgKOH/100ml) that 200ml furfural extraction unit is adopted back, add diluted de-acidying agent 0.6ml, then add 80ml distilled water, at 45 DEG C, fully stir 5min, after leaving standstill 20min, observe the interface conditions of furfural and the aqueous solution, get furfural and analyze acid number, test-results is in table 3.
As seen from Table 3, it is large that demulsifying agent consumption can make circulation furfural acidity reduce amplitude 20% ~ 40%, and furfural and aqueous solution interface clear not muddy.
From above-mentioned experimental result, the present invention has the following advantages:
(1) de-acidying agent adopted in method of the present invention, can not only effectively in and furfural acid in furfural and the acidic substance such as naphthenic acid, reduce the acid number of furfural, and the emulsion splitter in de-acidying agent can prevent furfural water system emulsification effectively, make the layering of furfural water system phase obvious, be separated both convenient, greatly can reduce the COD value of water.
(2) the de-acidying agent usage quantity that adopts of the present invention is few, in the furfural treatment aqueous solution system de-acidying agent concentration only need reach 30 ~ 40ppm can acid in effective elimination furfural.
(3) in the present invention, de-acidying agent usage quantity is few, and cost is low, reduces the cost of the depickling of furfural treatment.
(4) in the inventive method, de-acidying agent injects vacuum water sealed cans and water-soluble flow container respectively, so not only can improve deacidification effect, also alleviates corrosion and the coking of furfural extraction unit pumped vacuum systems water-sealed tank simultaneously, prevents water at the bottom of tank from taking out line and blocked by Jiao.
(5) de-acidying agent tank is located at a high position by the present invention, utilizing the effect of liquid self-pressure to complete de-acidying agent and injects, without the need to using de-acidying agent pump, having saved the energy.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the furfural device aqueous solution system of prior art.
Fig. 2 is the schematic diagram of furfural device aqueous solution system of the present invention.
Embodiment
Set forth content of the present invention in detail by the following examples, but following embodiment is just for setting forth content of the present invention, instead of restriction, therefore any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims.
embodiment one:
In furfural treatment technique, de-acidying agent softening water is diluted to the aqueous solution that concentration is 3%, pipeline section between the outlet valve and water-soluble flow container of vacuum tank 403/1 injects furfural treatment aqueous solution system, participate in furfural treatment, wherein de-acidying agent is by diethanolamine 50 grams, distilled water 30 grams and demulsifying agent 20 grams formation.Demulsifying agent is the combination of water-soluble demulsifier JH-3 and water-soluble demulsifier JH-5.
De-acidying agent is prepared as follows: diethanolamine 50 grams, and distilled water 30 grams joins in heating stirrer, heats to 50 DEG C and stirs 20min, then add demulsifying agent 20 grams, fully dissolves and follow-up continuing is warmed up to 60 DEG C of stirring 20min.
embodiment two:
With embodiment one unlike: de-acidying agent by diethanolamine 50 grams, distilled water 20 grams and demulsifying agent 30 grams formation.It is prepared as follows: take diethanolamine 50 grams, and distilled water 20 grams joins heating stirrer, is heated to 50 DEG C and stirs 20min, then add demulsifying agent 30 grams, fully dissolves and follow-up continuing is warmed up to 60 DEG C of stirring 20min.
embodiment three:
With embodiment one unlike: de-acidying agent by diethanolamine 45 grams, distilled water 20 grams and demulsifying agent 35 grams formation.It is prepared as follows: take diethanolamine 45 grams, and distilled water 20 grams joins heating stirrer, is heated to 50 DEG C and stirs 20min, then add demulsifying agent 35 grams, fully dissolves and follow-up continuing is warmed up to 60 DEG C of stirring 20min.
embodiment four:
With embodiment one unlike: de-acidying agent by diethanolamine 45 grams, distilled water 20 grams, demulsifying agent 35 grams and inhibiter vulkacit H 1.5 grams formation.It is prepared as follows: take diethanolamine 45 grams, and distilled water 20 grams joins heating stirrer, is heated to 50 DEG C of stirring 20min, then adds demulsifying agent 33.5 grams and vulkacit H 1.5 grams, fully dissolves and follow-up continuing is warmed up to 60 DEG C of stirring 20min.
embodiment five:
Furfural device aqueous solution system as shown in Figure 2, form primarily of de-acidying agent tank 411, vacuum tank 403/1, water-soluble flow container 405, drying tower 406, dehydration tower 407 and vacuum water sealed cans 410, water-soluble flow container 405 is connected with drying tower 406 and dehydration tower 407 respectively, stripping tower top 402 is out containing the solvent of large water gaging, enter in aqueous solution tank 405 after water cooler 4 cools and carry out layering, upper water solution water is pumped in dehydration tower 407 dewaters, and is returned in water-soluble flow container 405 after water cooler cooling by the furfural evaporated in point flow container 403/2.Lower floor's furfural is pumped to drying tower 406 through furfural and carries out drying, to be out recycled to after interchanger heat exchange water-soluble flow container 405 to be separated by the water that evaporates from tower top.Vacuum water sealed cans 410 are connected with vacuum tank 403/1.De-acidying agent tank 411 is arranged on the position higher than water-soluble flow container and vacuum water sealed cans 410, and concrete de-acidying agent tank 411 is arranged on 6 meters of eminences, and de-acidying agent tank and vacuum water sealed cans and water-soluble flow container position height difference are 3 meters.The solvent outlet of de-acidying agent tank 411 establishes two pipelines to be connected with water-soluble flow container 405 and vacuum water sealed cans 410 respectively thus to form two de-acidying agents to inject route.The de-acidying agent of de-acidying agent tank 411 divides two-way to inject water-soluble flow container 405 and vacuum water sealed cans 410 respectively.
In this embodiment, after de-acidying agent softening water is diluted to the aqueous solution of 3%, be placed in de-acidying agent tank 411, then under solution self-gravity action, injection vacuum water sealed cans 410 and water-soluble flow container 405 participate in furfural treatment process, until de-acidying agent concentration is 30ppm in furfural device aqueous solution system respectively.In whole treating processes, the temperature of water-soluble flow container 405 maintains 40 DEG C all the time.Wherein, de-acidying agent by diethanolamine 50 grams, distilled water 30 grams and demulsifying agent 20 grams formation.Demulsifying agent is the combination of water-soluble demulsifier JH-3 and water-soluble demulsifier JH-5.
embodiment six
With embodiment five unlike: after de-acidying agent softening water is diluted to the aqueous solution of 7%, inject vacuum water sealed cans 410 respectively and water-soluble flow container 405 participates in furfural treatment process, until de-acidying agent concentration is 35ppm in furfural device aqueous solution system.In whole treating processes, the temperature of water-soluble flow container 405 maintains 50 DEG C all the time.Wherein, de-acidying agent by diethanolamine 50 grams, distilled water 30 grams and demulsifying agent 20 grams formation.
embodiment seven
With embodiment five unlike: after de-acidying agent softening water is diluted to the aqueous solution of 10%, inject vacuum water sealed cans 410 respectively and water-soluble flow container 405 participates in furfural treatment process, until de-acidying agent concentration is 40ppm in furfural device aqueous solution system.In whole treating processes, the temperature of water-soluble flow container 405 maintains 55 DEG C all the time.Wherein, de-acidying agent by diethanolamine 50 grams, distilled water 30 grams and demulsifying agent 20 grams formation.
embodiment eight:
With embodiment five unlike: de-acidying agent softening water is diluted to the aqueous solution of 10%.De-acidying agent is made up of diethanolamine, distilled water, inhibiter and demulsifying agent.De-acidying agent preparation method is: take diethanolamine 45 grams, and distilled water 30 grams joins heating stirrer, is heated to 50 DEG C of stirring 20min, then adds demulsifying agent 20 grams and vulkacit H 5 grams, fully dissolves and follow-up continuing is warmed up to 60 DEG C of stirring 20min.
embodiment nine:
With embodiment eight unlike: de-acidying agent softening water is diluted to the aqueous solution of 9%.De-acidying agent is made up of diethanolamine 45 grams, distilled water 20 grams, demulsifying agent 30 grams and vulkacit H 5 grams.
embodiment ten:
With embodiment eight unlike: de-acidying agent softening water is diluted to the aqueous solution of 5%.De-acidying agent is made up of diethanolamine 45 grams, distilled water 10 grams, demulsifying agent 40 grams and vulkacit H 5 grams.
Claims (10)
1. can effectively reduce furfural acid number and a draining furfural treatment acid stripping method up to standard, in furfural treatment technique, de-acidying agent is with after softening water dilution, inject furfural treatment aqueous solution system, participate in furfural treatment process, it is characterized in that, described de-acidying agent comprises the component of following mass percent:
Organic amine 30% ~ 55%
Demulsifying agent 20% ~ 40%
Complex solvent 10% ~ 40%;
Described demulsifying agent is one or both combination in non-ionic polyacrylamide type emulsion splitter and small molecules branched structure polymkeric substance.
2. according to claim 1ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, described organic amine is one or both the combination in diethanolamine, trolamine.
3. according to claim 1ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, described non-ionic polyacrylamide type emulsion splitter is water-soluble demulsifier JH-3, and described small molecules branched structure polymkeric substance is water-soluble demulsifier JH-5.
4. according to claim 1ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, also comprise inhibiter, its mass percentage content in de-acidying agent is 1 ~ 5%.
5. according to claim 4ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, described inhibiter is vulkacit H.
6. can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard according to any one of claim 1-5, it is characterized in that, described de-acidying agent needs to be diluted to through softening water the aqueous solution that concentration is 3% ~ 10% before use.
7. according to claim 6ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, described de-acidying agent from de-acidying agent tank out after be divided into two sections through pipeline and inject furfural treatment aqueous solution systems, one section is injected vacuum water sealed cans, another section is injected into water-soluble flow container, and now described de-acidying agent tank is arranged at the position higher than water-soluble flow container and vacuum water sealed cans.
8. according to claim 6ly can effectively reduce furfural acid number and draining furfural treatment acid stripping method up to standard, it is characterized in that, the de-acidying agent concentration injected in furfural device is 30 ~ 40ppm; In depickling treating processes, the temperature of water-soluble flow container is kept to be 40 ~ 55 DEG C.
9. one kind implements the claims the furfural treatment aqueous solution system of 6 ~ 8 arbitrary described methods, comprise de-acidying agent tank, vacuum tank, water-soluble flow container, drying tower, dehydration tower and vacuum water sealed cans are formed, water-soluble flow container is connected with drying tower and dehydration tower respectively, the top gas outlet of drying tower and dehydration tower is connected to water-soluble flow container through interchanger and a point flow container respectively, described vacuum water sealed cans are connected with vacuum tank, it is characterized in that, described de-acidying agent tank is arranged at the position higher than water-soluble flow container and vacuum water sealed cans, its liquid outlet divides two pipelines to be connected with water-soluble flow container and vacuum water sealed cans respectively, form two-way de-acidying agent and inject route.
10. furfural treatment aqueous solution system according to claim 9, is characterized in that, described de-acidying agent tank and vacuum water sealed cans and water-soluble flow container position height difference are at least 3 meters.
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| CN112812083A (en) * | 2020-12-24 | 2021-05-18 | 山东林耀生物科技有限公司 | Furfural refining deacidification method capable of effectively reducing acid value of furfural and enabling drainage to reach standard |
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