CN1281843A - Improvement of 2-naphthol synthesis process - Google Patents
Improvement of 2-naphthol synthesis process Download PDFInfo
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- CN1281843A CN1281843A CN 99111810 CN99111810A CN1281843A CN 1281843 A CN1281843 A CN 1281843A CN 99111810 CN99111810 CN 99111810 CN 99111810 A CN99111810 A CN 99111810A CN 1281843 A CN1281843 A CN 1281843A
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Abstract
The present invention relates to an improvement on synthesis process of 2-naphthol, specially, it is a method using alkyl tertiary amine kerosene as extracting agent, extracting sodium beta-naphthalenesulfonate from neutralized mother liquor and returning it into naphthalene-blowing kettle for utilization. Said invented extraction process in implemented at normal temp. and under the condition of that pH is equal to 0.5-3, the ratio of extracting agent and neutralized mother liquor is 1:2-14(m.t), and the ratio of alkyl tertiary amine and kerosene is 1:0.1-1 (V), the NaOH is used to make reverse extraction at 70-95 deg.C, the ratio of alkali and extracting agent is 1:0.8-1.4 (m.t), and the ratio of alkali and hydrolysate in the reverse extraction liquor is 0.190-0.300:1 (mal). and the sodium beta-naphthalenesulfonate is returned into naphthalene-blowing kettle at 120-135 deg.C for utilization. The yield of sodium bate-naphthalenesulfonate is raised by about 10%, and COD being in waste water is reduced by about 90%.
Description
The present invention relates to a kind of improvement of beta naphthal synthesis technique, especially from and extraction sodium and it is returned the method for utilizing to the former synthesis process in the mother liquor.
As everyone knows, beta naphthal (2-Naphthol) is an important kind in the naphthalene system, is mainly used in synthetic dyestuff, pigment dyestuff and anti-aging agent etc." meticulous Organic Chemicals and intermediate handbook.Chemical Industry Press, 1998,3-107～3-108; " fine-chemical intermediate industrial production technology ".Dyestuffs industries press, 1996,184, announced that the main building-up process of beta naphthal is: naphthalene sulfonation, hydrolysis, blow processes such as naphthalene, neutralization, technological process is many, long flow path, quantity of three wastes is big, particularly in and mother liquor in the COD value up to 55000 mg/litre about, 1 ton of beta naphthal of every production, with produce about 8 cubic metres in and mother liquor, wherein mainly be sodium (β-position accounts for about 60%, and alpha-position accounts for about 20%) and inorganic salts etc.
Sodium is the important intermediate of Synthetic 2-naphthols, if in and contain a large amount of sodiums and do not recycled in the mother liquor, not only have influence on the yield and the production cost of beta naphthal, and contaminate environment seriously.It is reported that external-a little manufacturing enterprises just stop production because waste water pollution problem is difficult to solve.If utilize method of enrichment to explore solution route, but because the energy consumption height has the new three wastes to produce, organism and inorganic salt mix, and have influenced organic utilization.
The objective of the invention is to utilize extraction process from Synthetic 2-naphthols and in the mother liquor extraction sodium and it is turned back in the former beta naphthal synthesis process utilize.
Technical scheme of the present invention can be achieved like this:
With alkyl tertiary amine kerosene be extraction agent and beta naphthal in and mother liquor hybrid extraction under the situation of normal temperature (20～25 ℃), PH=0.5～3, extraction agent: in and mother liquor=1: 2～14 (m.t), static layering is separated, the extraction phase on recovery upper strata; In extraction phase, add 5%～20% sodium hydroxide solution, sodium hydroxide: extraction phase=1: 0.8～1.4 (m.t), being warming up to 70～95 ℃ and stripping, static layering is separated, reclaim the extraction agent on upper strata and the strip liquor (alkaliferous beta-naphthalenesulfonic-acid sodium solution, as follows) of lower floor; Make that sodium hydroxide and hydrolyzate mol ratio are 0.190～0.300: 1 in the strip liquor, in the time of 120～135 ℃, return and utilize to blowing in the naphthalene pot.
Technical scheme of the present invention also can be an extraction agent alkyl tertiary amine kerosin, and alkyl tertiary amine and kerosene volume ratio are 1: 0.1～1.
Technical scheme of the present invention can also be that the extraction agent that will reclaim recycles.
The present invention adopts above technical scheme to have the following advantages:
1, be extraction agent with the alkyl tertiary amine kerosin, sodium hydroxide solution is that strippant reclaims sodium from the beta naphthal synthetic He in the mother liquor, and return to blowing in the naphthalene pot and recycle to contain alkali beta-naphthalenesulfonic-acid sodium solution form, finally realize raising beta naphthal yield about 10%, reduced the purpose of beta naphthal production cost.
2, in the extracting phase COD value by 55000 original mg/litre about, be reduced to below 5000 mg/litre, after sedimentation is handled,,, alleviate environmental pollution to reach discharge index with other factory effluent comprehensive treating processs.
Therefore, the present invention sets about from technology itself, from beta naphthal He in the mother liquor, reclaim sodium, substantially do not changing under the condition of the former synthesis technique of beta naphthal, it is returned to blowing in the naphthalene pot utilize, simultaneously, make its waste water obtain administering, solved and wanted for a long time to solve and unsolved a great problem.
Accompanying drawing improves synoptic diagram for the beta naphthal synthesis technique, and its dotted line right side is the original production schematic flow sheet; The strip liquor that the dotted line left side recycles, reclaims for the extraction agent of newly-installed extraction, reextraction process and recovery returns the synoptic diagram that utilizes process in the naphthalene pot to blowing.
Alkyl tertiary amine, its general formula are R3(R is alkyl: C to NnH
2n+1), proportion is about 0.8, Water insoluble, be slightly soluble in methyl alcohol.
Kerosene is C11～C
17The high-boiling hydrocarbon mixture, take saturated hydrocarbons as main, Jilin chemical industry Limited company's oil plant is produced this product, and relative density is 0.800.
The present invention utilizes extraction, extracts sodiumβ-naphthalenesulfonate from beta naphthal He in the mother liquor, and is main Based on alkyl tertiary amine in acid medium can with in and in the mother liquor sodiumβ-naphthalenesulfonate generate water-fast Salt, thus reach the purpose of separating with raffinate phase (waste water), strip with NaOH again, Separating and recovering extractant recirculation is used. When alkyl tertiary amine is done the extractant use, must be with kerosene by certain Dilution proportion, its strip liquor can turn back to blow in the naphthalene pot and utilize.
In order to further specify the principle of above-mentioned extraction, reextraction, now show it with chemical equation:
1, extraction:
2, strip:
The strip liquor that the present invention reclaims can return to blowing in the naphthalene pot and utilize, and one reclaims sodiumβ-naphthalenesulfonate; Two use excessive aqueous slkali as part material alkali.
Embodiment 1:
(1), extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, 41 milliliters of accent of the sulfuric acid pH value that stirs adding 98% down is 1.5, add 225 milliliters of three octyl tertiary amines and 25 kerosins then, thorough mixing, pour into then in the separating funnel, static layering is separated.Reclaiming the upper strata extraction phase is 275 milliliters, and lower floor's extracting phase COD value is 2378.51mg/L, after sedimentation is handled, delivers to composite wastewater treatment plant and handles back up to standard discharging.
300 milliliters in the sodium hydroxide of adding 5% in 275 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 70 ℃, pour in the separating funnel, static layering is separated, reclaim 248 milliliters of the extraction agents in upper strata (can be recycled), lower floor's strip liquor is 360 milliliters, basicity 2%, and proportion is 1.1 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g adding blows in the naphthalene still, to above-mentioned basicity is to add when adding 95% sodium hydroxide, 16.9 gram dissolving backs at 128 ℃ in 2% the strip liquor to blow in the naphthalene pot, feeds water vapor and blows away naphthalene, and the naphthalene that blows out reclaims with the cold water spray, blow that volume of material is 800 milliliters behind the naphthalene, acidity is 16%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1400 milliliters down in 85 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 37 ℃ of filtrations, drain, get paste 843 grams, moisture content 19%, beta-naphthalenesulfonic-acid sodium content are 99.6%.
Embodiment 2:
(1) extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, 45 milliliters in the sulfuric acid of adding 98% under stirring, transferring pH value is 0.5 to add 165 milliliters of 250 milliliters of the extraction agents that example 1 reclaims and the kerosene of adding then, thorough mixing, pour into then in the separating funnel, static layering is separated.Reclaiming the upper strata extraction phase is 450 milliliters.Lower floor's extracting phase COD value is 1803.38mg/L, delivers to composite wastewater treatment plant and handle back up to standard discharging after sedimentation is handled.
440 milliliters in the sodium hydroxide of adding 7% in 450 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 80 ℃, pour in the separating funnel, static layering is separated, reclaim 410 milliliters of the extraction agents in upper strata (can be recycled), lower floor's strip liquor is 500 milliliters, basicity 1.9%, and proportion is 1.09 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g adding blows in the naphthalene pot, with above-mentioned basicity is that 500 milliliters of 1.9% strip liquors are added 95% sodium hydroxide, 10.2 grams, after being concentrated into 260 milliliters, in the time of 135 ℃, add and blow in the naphthalene pot, feed water vapor and blow away naphthalene, the naphthalene that blows out reclaims with cold water spray, blows that volume of material is 850 milliliters behind the naphthalene, and acidity is 15.5%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1400 milliliters down in 90 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 40 ℃ of filtrations, drain, get paste 835 grams, moisture content 18%, its beta-naphthalenesulfonic-acid sodium content is 99.7%.
Embodiment 3:
(1) extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, 43 milliliters in the sulfuric acid of adding 98% under stirring, transferring pH value is 1, the mixture that adds 210 milliliters of three butane group tertiary amines and 100 milliliters of kerosene, thorough mixing is poured in the separating funnel then, and static layering is separated.Reclaiming the upper strata extraction phase is 340 milliliters.Lower floor's extracting phase COD value is 3120mg/L, delivers to composite wastewater treatment plant and handle back up to standard discharging after sedimentation is handled.
400 milliliters in the sodium hydroxide of adding 8% in 340 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 95 ℃, pour in the separating funnel, static layering is separated, reclaim 308 milliliters of the extraction agents in upper strata (can be recycled), 450 milliliters of lower floor's strip liquors, basicity are 3%, and proportion is 1.25 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g and add and to blow in the naphthalene pot, is that 3% strip liquor is added 95% sodium hydroxide, 5 grams for 450 milliliters with above-mentioned basicity, adds in the time of 135 ℃ and blows in the naphthalene pot, feed water vapor and blow away naphthalene, the naphthalene that blows out reclaims with cold water spray, blows that volume of material is 860 milliliters behind the naphthalene, and acidity is 15.8%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1410 milliliters down in 87 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 40 ℃ of filtrations, drain, get paste 842 grams, moisture content 19.5%, its beta-naphthalenesulfonic-acid sodium content is 99.6%.
Embodiment 4:
(1) extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, 45 milliliters in the sulfuric acid of adding 98% under stirring, transferring pH value is 0.5 to add 525 milliliters of 308 milliliters of the extraction agents that example 3 reclaims and 415 milliliters of the three butane group tertiary amines of adding and kerosene then, thorough mixing, pour into then in the separating funnel, static layering is separated.Reclaiming the upper strata extraction phase is 1275 milliliters.Lower floor's extracting phase COD value is 1091.8mg/L, delivers to composite wastewater treatment plant and handle back up to standard discharging after sedimentation is handled.
330 milliliters in the sodium hydroxide of adding 20% in 1275 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 85 ℃, pour in the separating funnel, static layering is separated, reclaim 1245 milliliters of the extraction agents in upper strata (can be recycled), lower floor's strip liquor is 380 milliliters, basicity 5.9%, and proportion is 1.3 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g and add and to blow in the naphthalene pot, is 380 milliliters of 5.9% strip liquors with above-mentioned basicity, adds in the time of 120 ℃ and blows in the naphthalene pot, feed water vapor and blow away naphthalene, the naphthalene that blows out reclaims with cold water spray, blows that volume of material is 850 milliliters behind the naphthalene, and acidity is 15.2%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1400 milliliters down in 90 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 40 ℃ of filtrations, drain, get paste 834 grams, moisture content 19%, its beta-naphthalenesulfonic-acid sodium content is 99.5%.
Embodiment 5:
(1) extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, 38 milliliters in the sulfuric acid of adding 98% under stirring, transferring pH value is 2, the mixture that adds 400 milliliter of three bay alkyl tertiary amine and 100 milliliters of kerosene, thorough mixing is poured in the separating funnel then, and static layering is separated.Reclaiming the upper strata extraction phase is 550 milliliters.Lower floor's extracting phase COD value is 2350mg/L, delivers to composite wastewater treatment plant and handle back up to standard discharging after sedimentation is handled.
240 milliliters in the sodium hydroxide of adding 15% in 550 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 88 ℃, pour in the separating funnel, static layering is separated, reclaim 495 milliliters of the extraction agents in upper strata (can be recycled), 290 milliliters of lower floor's strip liquors, basicity are 7.1%, and proportion is 1.35 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g and add and to blow in the naphthalene pot, is 290 milliliters of 7.1% strip liquors with above-mentioned basicity, adds in the time of 125 ℃ and blows in the naphthalene pot, feed water vapor and blow away naphthalene, the naphthalene that blows out reclaims with cold water spray, blows that volume of material is 870 milliliters behind the naphthalene, and acidity is 15.1%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1450 milliliters down in 87 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 35 ℃ of filtrations, drain, get paste 850 grams, moisture content 20%, its beta-naphthalenesulfonic-acid sodium content is 99.75%.
Embodiment 6:
(1) extraction and reextraction
Get in the beta naphthal and the post output in and 2500 milliliters in mother liquor (proportion is 1.1), pour in the beaker, stir and add 40 milliliters in 98% sulfuric acid down, transferring pH value is 1.8 add 495 milliliters of the extraction agents that example 5 reclaims then, add 200 milliliters of three bay alkyl tertiary amines again, 100 milliliters of kerosene, and thorough mixing is poured in the separating funnel then, and static layering is separated.Reclaiming the upper strata extraction phase is 850 milliliters.Lower floor's extracting phase COD value is 2589mg/L, delivers to composite wastewater treatment plant and handle back up to standard discharging after sedimentation is handled.
350 milliliters in the sodium hydroxide of adding 10% in 850 milliliters of extraction phases (proportion 0.92) of above-mentioned recovery, stirring is warming up to 90 ℃, pour in the separating funnel, static layering is separated, reclaim 796 milliliters of the extraction agents in upper strata (can be recycled), lower floor's strip liquor is 760 milliliters, basicity 5.8%, and proportion is 1.3 can return to blow in the naphthalene pot and utilize.
(2) blow naphthalene, neutralization, filtration
Getting hydrolyzate 846g and add and to blow in the naphthalene pot, is 400 milliliters of 5.8% strip liquors with above-mentioned basicity, adds in the time of 130 ℃ and blows in the naphthalene pot, feed water vapor and blow away naphthalene, the naphthalene that blows out reclaims with cold water spray, blows that volume of material is 920 milliliters behind the naphthalene, and acidity is 15.5%.Slowly add sodium sulfite aqueous solution (concentration 15%) 1440 milliliters down in 90 ℃ of stirrings, feed steam and catch up with sulfurous gas, the sulfurous gas that blows out absorbs with dilute alkaline soln; Be cooled to 38 ℃ of filtrations, drain, get paste 854 grams, moisture content 20.5%, its beta-naphthalenesulfonic-acid sodium content is 99.67%.
The beta naphthal intermediate sodium that adopts former technology to make, its yield is about 85%, improve the 3-sodium naphthalene sulfonate that back technology makes and adopt, its yield can improve about 10%, with improving the sodium that back technology makes, the betanaphthol sodium that behind alkali fusion, makes, its alkali fusion index is consistent with the betanaphthol sodium index that former technology makes:
The existing technic index of the former technic index of quality index
Free alkali 2～3% 2～3%
S-WAT 35% 35%
Beta naphthal 44% 44%
Claims (3)
1, a kind of improvement of beta naphthal synthesis technique mainly comprises the naphthalene sulfonation, and naphthalene is blown in hydrolysis, and processes such as neutralization is characterized in that:
A. with the alkyl tertiary amine kerosin be extraction agent and beta naphthal in and mother liquor, hybrid extraction under the situation of normal temperature (20～25 ℃), PH=0.5～3, extraction agent: in and mother liquor=1: 2～14 (m.t), static layering is separated, and reclaims the upper strata extraction phase,
B. in extraction phase, add concentration and be 5%～20% sodium hydroxide solution, sodium hydroxide: extraction phase=1: 0.8～1.4 (m.t), being warming up to 70～95 ℃ after the mixing strips, static layering is separated, reclaim the extraction agent on upper strata, strip liquor (alkaliferous beta-naphthalenesulfonic-acid sodium solution) with lower floor
C. making sodium hydroxide and hydrolyzate mol ratio in the strip liquor of recovery is 0.190-0.300: 1, and return to blowing in the naphthalene pot in 120～135 ℃ and to utilize.
2, the improvement of beta naphthal synthesis technique according to claim 1 is characterized in that the alkyl tertiary amine of extraction agent and kerosene volume ratio are 1: 0.1～1.
3,, it is characterized in that extraction agent alkyl tertiary amine kerosin can be recycled according to the improvement of claim 1 or the described beta naphthal synthesis technique of claim 2.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99111810 CN1281843A (en) | 1999-07-21 | 1999-07-21 | Improvement of 2-naphthol synthesis process |
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|---|---|---|---|
| CN 99111810 CN1281843A (en) | 1999-07-21 | 1999-07-21 | Improvement of 2-naphthol synthesis process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310880C (en) * | 2004-01-18 | 2007-04-18 | 李阳 | Improved process for preparing 2-sodium naphthalenesulfonate in production of beta-naphthol |
| CN101230025A (en) * | 2008-02-22 | 2008-07-30 | 广东纺织职业技术学院 | Extractive recovery method for aryl sulfonic acid salt in waste water |
| CN102936051A (en) * | 2012-11-19 | 2013-02-20 | 上海百菲特环保科技有限公司 | Process for treating dinaphthol wastewater by using complexation extraction method |
| CN103232087A (en) * | 2013-05-17 | 2013-08-07 | 新昌德力石化设备有限公司 | Method for continuously treating sulfonic acid wastewater |
| CN103626637A (en) * | 2013-12-11 | 2014-03-12 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of 2-naphthol |
| CN104628608A (en) * | 2015-02-16 | 2015-05-20 | 曲靖众一合成化工有限公司 | Method and device for blowing naphthalene via gas stripping by using tower type negative pressure continuous inert gas |
-
1999
- 1999-07-21 CN CN 99111810 patent/CN1281843A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310880C (en) * | 2004-01-18 | 2007-04-18 | 李阳 | Improved process for preparing 2-sodium naphthalenesulfonate in production of beta-naphthol |
| CN101230025A (en) * | 2008-02-22 | 2008-07-30 | 广东纺织职业技术学院 | Extractive recovery method for aryl sulfonic acid salt in waste water |
| CN102936051A (en) * | 2012-11-19 | 2013-02-20 | 上海百菲特环保科技有限公司 | Process for treating dinaphthol wastewater by using complexation extraction method |
| CN103232087A (en) * | 2013-05-17 | 2013-08-07 | 新昌德力石化设备有限公司 | Method for continuously treating sulfonic acid wastewater |
| CN103626637A (en) * | 2013-12-11 | 2014-03-12 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of 2-naphthol |
| CN103626637B (en) * | 2013-12-11 | 2014-12-24 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of 2-naphthol |
| CN104628608A (en) * | 2015-02-16 | 2015-05-20 | 曲靖众一合成化工有限公司 | Method and device for blowing naphthalene via gas stripping by using tower type negative pressure continuous inert gas |
| CN104628608B (en) * | 2015-02-16 | 2016-11-16 | 曲靖众一合成化工有限公司 | A kind of tower negative pressure continuous noble gas air stripping blows naphthalene method and device thereof |
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