CN1861594A - Purifying process of poor quality cyclo butyl sulfone - Google Patents
Purifying process of poor quality cyclo butyl sulfone Download PDFInfo
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- CN1861594A CN1861594A CN 200510069338 CN200510069338A CN1861594A CN 1861594 A CN1861594 A CN 1861594A CN 200510069338 CN200510069338 CN 200510069338 CN 200510069338 A CN200510069338 A CN 200510069338A CN 1861594 A CN1861594 A CN 1861594A
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- exchange resin
- tetramethylene sulfone
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Abstract
A process for purifying the poor-grade sulfolane features that the sulfolane flows through anionic exchange layer continuously while measuring its pH value and controlling its flow according to the measured pH value.
Description
Technical field
The present invention relates to the purifying method of inferior sulfolane, relate more specifically to use the inferior sulfolane purifying method of ion-exchange.
Background technology
At present, the industrial tetramethylene sulfone that generally uses owing to tetramethylene sulfone oxidative degradation in use produces acidic substance, makes the potential of hydrogen of tetramethylene sulfone change as the extractive solvent of aromatic hydrocarbons, and the pH value constantly descends, and the character of tetramethylene sulfone is variation gradually also.Inferior sulfolane can cause heavy corrosion to equipment, and in order to prevent the poor qualityization of tetramethylene sulfone, the industrial method of generally using ion-exchange purifies inferior sulfolane and regenerates.
A kind of renovation process of inferior sulfolane is disclosed as CN1230545A, this method with inferior sulfolane under 25-40 ℃, with 1.0-5.0 rice/hour linear velocity flow through anion exchange resin layer.This method flows through the effluent of anion exchange resin layer by mensuration pH value is judged the effect of ion-exchange, when the treatment capacity of anionite-exchange resin reaches its saturated exchange capacity, could continue after anionite-exchange resin need be regenerated to use.But this method is that basis for estimation is operated with the experimental determination data of off-line sampling, therefore can't change the flow of on-line Control tetramethylene sulfone according to the potential of hydrogen of tetramethylene sulfone, causes the relatively poor or wastage of material of decontamination effect improving easily.
Summary of the invention
The objective of the invention is to overcome the problem that aforesaid method can't change on-line Control tetramethylene sulfone flow according to the potential of hydrogen of tetramethylene sulfone, a kind of purifying method that can change the inferior sulfolane of on-line Control tetramethylene sulfone flow according to the tetramethylene sulfone potential of hydrogen is provided.
The purifying method of inferior sulfolane provided by the invention comprises makes tetramethylene sulfone flow through anion exchange resin layer continuously, wherein this method is provided with an online pH meter at least on the path of the tetramethylene sulfone that flows through anion exchange resin layer, the pH value of on-line determination tetramethylene sulfone is according to the flow of the pH value control tetramethylene sulfone of measuring.
Because pH value can on-line determination, therefore can when regenerate or change according to the timely judgement of the online pH value that records anionite-exchange resin.The pH value that records when online pH meter can provide control signal automatically when reaching set(ting)value and operate accordingly or manually operate accordingly, thereby has avoided unnecessary operation and supplies consumption, the problem of the relatively poor and wastage of material of decontamination effect improving can not occur.Therefore, saved raw material, reduced cost, and be more prone to realize automated operation, enhanced productivity.
Description of drawings
Fig. 1 is the synoptic diagram of principle of the purifying method of inferior sulfolane provided by the invention;
Fig. 2 is the synoptic diagram of principle of the purifying method of inferior sulfolane provided by the invention;
Fig. 3 is the synoptic diagram of principle of the purifying method of inferior sulfolane provided by the invention.
Embodiment
According to method provided by the invention, the pH value of described inferior sulfolane is generally 3-5 less than 7.5; PH value through tetramethylene sulfone after the ion-exchange is increased to more than 7.5, is generally 7.5-10.0, and therefore the pH value of tetramethylene sulfone changes before and after ion-exchange.
As shown in Figure 1, when according to method provided by the invention inferior sulfolane being purified, at first Open valve 13, and tetramethylene sulfone 1 is flow through anion exchange resin layer 6, carry out ion-exchange.The path of the tetramethylene sulfone 2 after flowing through anion exchange resin layer 6 promptly is provided with online pH meter 7 on the pipeline 10, mensuration flows through the pH value pH1 of the tetramethylene sulfone 2 after the anion exchange resin layer 6.When the value of pH1 is a value less than 7.5, be preferably a value less than 6.0, more preferably during 5.0-6.0 value, adopt artificial or automatic control device valve-off 13, stop tetramethylene sulfone 1 and enter anion exchange resin layer 6.While Open valve 14, making a certain amount of regeneration soln 3 enter anion exchange resin layer 6 regenerates, regeneration soln has been crossed anion exchange resin layer 6 Open valve 15 afterwards, and with deionized water 4 drip washing, described regeneration soln and deionized water are discharged from pipeline 12.
As shown in Figure 2, this method is the passage of the tetramethylene sulfone before flowing through anion exchange resin layer 61 further, and online pH meter 8 promptly is set on the pipeline 11, and mensuration flows through the pH value pH2 of the tetramethylene sulfone 1 before the anion exchange resin layer 6.When according to method provided by the invention inferior sulfolane being purified, at first Open valve 13, and tetramethylene sulfone 1 is flow through anion exchange resin layer 6, carry out ion-exchange.Obtain the pH1 of pH meter 7 mensuration and the pH2 that pH meter 8 is measured respectively, when the difference of pH1 and pH2 is the value of 1-5.5, when being preferably value of 1-3.0, adopt artificial or automatic control device valve-off 13, stop tetramethylene sulfone 1 and enter anion exchange resin layer 6.Open valve 14 makes a certain amount of regeneration soln 3 enter anion exchange resin layer 6 and regenerates simultaneously, and regeneration soln has been crossed anion exchange resin layer 6 Open valve 15 afterwards, with deionized water 4 drip washing.Described regeneration soln and deionized water are discharged from pipeline 12.
As shown in Figure 3, this method can also promptly be provided with online pH meter 9 further at described regeneration soln and the effusive passage of deionized water on the pipeline 12, measures the pH value pH3 of eluate (regeneration soln and deionized water) 5.When pH3 is value of 7-8, adopt artificial or automatic control device valve-off 15, stop the resin regeneration program.Open valve 13 makes tetramethylene sulfone 1 flow through anion exchange resin layer 6 simultaneously, and inferior sulfolane purifies.So just realized the on-line Control that tetramethylene sulfone purifies.Wherein, described regeneration soln can be in the alkali metal hydroxide aqueous solution one or more, is preferably the sodium hydroxide solution of 3-4 weight %; The volumetric usage of the sodium hydroxide solution of 3-4 weight % is preferably 4-5 times of anionite-exchange resin volume.
According to tetramethylene sulfone purifying method provided by the invention, online pH meter can be measured the pH value of liquid continuously, the pH value of also can intermittent type ground measuring liquid, promptly at regular intervals as on-line determination such as 12 hours, 24 hours, 48 hours once, preferably measure the pH value of liquid in a preferred embodiment of the invention continuously.
According to tetramethylene sulfone purifying method provided by the invention, utilize pH value control tetramethylene sulfone flow can adopt the artificial method, perhaps adopt the method for automatic control device control, preferably adopt the method for automatic control device control.Adopt the method for the flow of automatic control device controlled liq can adopt any existing method, for example, adopt the valve of the flow passage of rly. control tetramethylene sulfone, flow or do not flow with the control tetramethylene sulfone, and the size of flow.
Described pH meter can be the online pH meter of various models, as long as its testing range and tolerance range meet the demands.Usually, the testing range of pH meter is 0-14, and tolerance range is 0.01.Described online pH meter can be commercially available, as the industrial on-line measurement instrument of the pH296 of Hangzhou Ke Sheng mechanical ﹠ electronic equipment corporation, Ltd production, 2000pH industry on-line measurement instrument, pH170 industry on-line measurement instrument etc.
The kind of the anionite-exchange resin that is adopted in the tetramethylene sulfone purifying method provided by the invention and using method are for as well known to those skilled in the art.
Anionite-exchange resin is weak base anion-exchange resin, strongly basic anion exchange resin or gel strongly basic anion exchange resin.Be preferably the polystyrene weak base anion-exchange resin, as-NH
2,-N (CH
3)
2Type.
Commercially available anionite-exchange resin needs to make it become the OH type by the storage type through pre-treatment before use.Pretreated step is at room temperature soaking more than 24 hours with deionized water commercially available anionite-exchange resin, again with volume be the anionite-exchange resin volume 4-5 doubly, concentration is that the sodium hydroxide solution of 3-4 weight % is converted to the OH type with resin, be about 1 hour switching time, is 7-8 with deionized water drip washing resin to the pH value of elutriant then.
The weight ratio that the treatment capacity of described tetramethylene sulfone should be controlled at tetramethylene sulfone and anionite-exchange resin is 10-160: 1, be preferably 10-120: 1.Then lose activity when the treatment capacity of described anionite-exchange resin reaches its exchange capacity, can continue to use through regeneration, the regenerated method be identical with above-mentioned pretreated method.
Tetramethylene sulfone flows through the linear flow speed of anionite-exchange resin and the temperature of ion-exchange has been as well known to those skilled in the art.Usually, described linear flow speed be 1-10 rice/hour, be preferably 3-8 rice/hour, temperature is 20-80 ℃, is preferably 25-40 ℃.
To the present invention be described in more detail by specific embodiment below.
This embodiment is used to illustrate the purifying method of tetramethylene sulfone provided by the present invention.
Get commercially available weakly alkaline polystyrene-N (CH
3)
2(Shanghai Resin Factory produces type anionite-exchange resin, the D709-S type), soaked 24 hours with deionized water, be loaded in the glass column, with the NaOH solution of 4 weight % of 4 times of volumes by anionite-exchange resin 1 hour, being converted into the OH type, is to stop drip washing at 7.1 o'clock with deionized water drip washing anionite-exchange resin to pH value then.
As shown in Figure 1, at first Open valve 13, and tetramethylene sulfone 1 under 30 ℃, by above-mentioned switched anion exchange resin layer 6, is carried out ion-exchange with 6 meters/hour linear velocities.The path of the tetramethylene sulfone 2 after flowing through anion exchange resin layer 6 promptly is provided with online pH meter 7 on the pipeline 10, mensuration flows through the pH value pH1 of the tetramethylene sulfone 2 after the anion exchange resin layer 6.When the value of pH1 is 6.0,, stops tetramethylene sulfone 1 and enter anion exchange resin layer 6 by relay-set automatic-closing valve 13.Simultaneously by the automatic Open valve 14 of relay-set, make regeneration soln 3 (volume is the NaOH solution of 4 weight % of 4 times of anionite-exchange resin volumes) enter anion exchange resin layer 6, Open valve 15 then, with deionized water 4 drip washing, described regeneration soln and deionized water are discharged from pipeline 12.
This embodiment is used to illustrate the purifying method of tetramethylene sulfone provided by the present invention.
Use with embodiment 1 in identical method anionite-exchange resin is carried out pre-treatment.
As shown in Figure 2, at first Open valve 13, and tetramethylene sulfone 1 under 35 ℃, by above-mentioned switched anion exchange resin layer 6, is carried out ion-exchange with 4 meters/hour linear velocities.The path of the tetramethylene sulfone 2 after flowing through anion exchange resin layer 6 promptly is provided with online pH meter 7 on the pipeline 10, mensuration flows through the pH value pH1 of the tetramethylene sulfone 2 after the anion exchange resin layer 6.The passage of the tetramethylene sulfone 1 before flowing through anion exchange resin layer 6 promptly is provided with online pH meter 8 on the pipeline 11 simultaneously, and mensuration flows through the pH value pH2 of the tetramethylene sulfone 1 before the anion exchange resin layer 6.The pH value pH2 that online pH meter 8 is measured tetramethylene sulfone 1 is 4.5, when the difference of pH1 and pH2 is 1.0, by relay-set automatic-closing valve 13, stops tetramethylene sulfone 1 and enters anion exchange resin layer 6.While Open valve 14, make regeneration soln 3 (volume is the NaOH solution of 4 weight % of 5 times of anionite-exchange resin volumes) enter anion exchange resin layer 6, Open valve 15 then, and with deionized water 4 drip washing, described regeneration soln and deionized water are discharged from pipeline 12.
As shown in Figure 3,, online pH meter 9 is set on the pipeline 12 promptly, measures the pH value pH3 of eluate (regeneration soln and deionized water) 5 at described regeneration soln and the effusive passage of deionized water.When pH3 was 7.8, by relay-set automatic-closing valve 15, Open valve 13 made tetramethylene sulfone 1 flow through anion exchange resin layer 6 simultaneously, and inferior sulfolane purifies.
This embodiment is used to illustrate the purifying method of tetramethylene sulfone provided by the present invention.
Use with embodiment 1 in identical method anionite-exchange resin is carried out pre-treatment.
As shown in Figure 1, at first Open valve 13, and tetramethylene sulfone 1 under 40 ℃, by above-mentioned switched anion exchange resin layer 6, is carried out ion-exchange with 7 meters/hour linear velocities.The path of the tetramethylene sulfone 2 after flowing through anion exchange resin layer 6 promptly is provided with online pH meter 7 on the pipeline 10, mensuration flows through the pH value pH1 of the tetramethylene sulfone 2 after the anion exchange resin layer 6.When the value of pH1 is 5.5,, stops tetramethylene sulfone 1 and enter anion exchange resin layer 6 by relay-set automatic-closing valve 13.While Open valve 14, make regeneration soln 3 (volume is the NaOH solution of 4 weight % of 4 times of anionite-exchange resin volumes) enter anion exchange resin layer 6, Open valve 15 then, and with deionized water 4 drip washing, described regeneration soln and deionized water are discharged from pipeline 12.
As shown in Figure 3,, online pH meter 9 is set on the pipeline 12 promptly, measures the pH value pH3 of eluate (regeneration soln and deionized water) 5 at described regeneration soln and the effusive passage of deionized water.When pH3 was 7.2, by relay-set automatic-closing valve 15, Open valve 13 made tetramethylene sulfone 1 flow through anion exchange resin layer 6 simultaneously, and inferior sulfolane purifies.
This embodiment is used to illustrate the purifying method of tetramethylene sulfone provided by the present invention.
Use with embodiment 1 in identical method anionite-exchange resin is carried out pre-treatment.
As shown in Figure 2, at first Open valve 13, and tetramethylene sulfone 1 under 35 ℃, by above-mentioned switched anion exchange resin layer 6, is carried out ion-exchange with 3 meters/hour linear velocities.The path of the tetramethylene sulfone 2 after flowing through anion exchange resin layer 6 promptly is provided with online pH meter 7 on the pipeline 10, mensuration flows through the pH value pH1 of the tetramethylene sulfone 2 after the anion exchange resin layer 6.The passage of the tetramethylene sulfone 1 before flowing through anion exchange resin layer 6 promptly is provided with online pH meter 8 on the pipeline 11 simultaneously, and mensuration flows through the pH value pH2 of the tetramethylene sulfone 1 before the anion exchange resin layer 6.The pH value pH2 that online pH meter 8 is measured tetramethylene sulfone 1 is 3.2, when the difference of pH1 and pH2 is 2.5, by relay-set automatic-closing valve 13, stops tetramethylene sulfone 1 and enters anion exchange resin layer 6.While Open valve 14, make regeneration soln 3 (volume is the NaOH solution of 3 weight % of 4 times of anionite-exchange resin volumes) enter anion exchange resin layer 6, Open valve 15 then, and with deionized water 4 drip washing, described regeneration soln and deionized water are discharged from pipeline 12.
As shown in Figure 3,, online pH meter 9 is set on the pipeline 12 promptly, measures the pH value pH3 of eluate (regeneration soln and deionized water) 5 at described regeneration soln and the effusive passage of deionized water.When pH3 was 7.5, by relay-set automatic-closing valve 15, Open valve 13 made tetramethylene sulfone 1 flow through anion exchange resin layer 6 simultaneously, and inferior sulfolane purifies.
Claims (13)
1, a kind of purifying method of inferior sulfolane comprises and makes tetramethylene sulfone flow through anion exchange resin layer continuously, it is characterized in that, this method is provided with an online pH meter on the path of the tetramethylene sulfone after flowing through anion exchange resin layer at least, the pH value of on-line determination tetramethylene sulfone is according to the flow of the pH value of The real time measure control tetramethylene sulfone.
2, method according to claim 1 is characterized in that, the pH value of described inferior sulfolane is less than 7.5, and the pH value that flows through the tetramethylene sulfone after the anion exchange resin layer is greater than 7.5.
3, method according to claim 2 is characterized in that, the pH value of described inferior sulfolane is 3-5, and the pH value that flows through the tetramethylene sulfone after the anion exchange resin layer is 7.5-10.0.
4, method according to claim 1, it is characterized in that, flow through tetramethylene sulfone pH value after the anion exchange resin layer for the time when what described online pH meter recorded less than value of 6.0, adopt artificial or automatic control device makes tetramethylene sulfone stop to flow through anion exchange resin layer, carry out the regeneration of anionite-exchange resin.
5, method according to claim 1 is characterized in that, this method further is provided with an online pH meter, the pH value of on-line determination inferior sulfolane on the path of the tetramethylene sulfone before flowing through anion exchange resin layer.
6, method according to claim 5, it is characterized in that, when the difference that flows through the tetramethylene sulfone pH value before and after the anion exchange resin layer that records when described online pH meter is value of 1-3.0, adopt artificial or automatic control device makes tetramethylene sulfone stop to flow through anion exchange resin layer, carry out the regeneration of anionite-exchange resin.
According to claim 4 or 6 described methods, it is characterized in that 7, the regeneration of described anionite-exchange resin comprises makes regeneration soln contact with anion exchange resin layer, uses deionized water drip washing then.
8, method according to claim 7, it is characterized in that, this method further is provided with an online pH meter on regeneration soln and the effusive path of deionized water, when the pH value that records is value of 7-8, adopt artificial or automatic control device to stop the regeneration of anionite-exchange resin, make tetramethylene sulfone flow through anion exchange resin layer.
According to claim 7 or 8 described methods, it is characterized in that 9, described regeneration soln is one or more in the alkali metal hydroxide aqueous solution.
10, method according to claim 1 is characterized in that, the linear flow speed that tetramethylene sulfone flows through anion exchange resin layer for 1-10 rice/hour, temperature is 20-80 ℃.
11, method according to claim 10 is characterized in that, the linear flow speed that tetramethylene sulfone flows through anion exchange resin layer for 3-8 rice/hour, temperature is 25-40 ℃.
According to any described method among the claim 1-11, it is characterized in that 12, described anionite-exchange resin is weak base anion-exchange resin, strongly basic anion exchange resin or gel strongly basic anion exchange resin.
13, method according to claim 12 is characterized in that, described anionite-exchange resin is the polystyrene weak base anion-exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510069338 CN1861594A (en) | 2005-05-13 | 2005-05-13 | Purifying process of poor quality cyclo butyl sulfone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510069338 CN1861594A (en) | 2005-05-13 | 2005-05-13 | Purifying process of poor quality cyclo butyl sulfone |
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| CN1861594A true CN1861594A (en) | 2006-11-15 |
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|---|---|---|---|
| CN 200510069338 Pending CN1861594A (en) | 2005-05-13 | 2005-05-13 | Purifying process of poor quality cyclo butyl sulfone |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240132A (en) * | 2012-02-10 | 2013-08-14 | 苏州艾科水处理设备工程有限公司 | Inferior sulfolane regenerator |
| CN109365009A (en) * | 2018-11-20 | 2019-02-22 | 杭州多能环保科技有限公司 | A kind of preparation method of the ion exchange resin for sulfolane purification |
-
2005
- 2005-05-13 CN CN 200510069338 patent/CN1861594A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240132A (en) * | 2012-02-10 | 2013-08-14 | 苏州艾科水处理设备工程有限公司 | Inferior sulfolane regenerator |
| CN103240132B (en) * | 2012-02-10 | 2015-06-03 | 苏州艾科水处理设备工程有限公司 | Inferior sulfolane regenerator |
| CN109365009A (en) * | 2018-11-20 | 2019-02-22 | 杭州多能环保科技有限公司 | A kind of preparation method of the ion exchange resin for sulfolane purification |
| CN109365009B (en) * | 2018-11-20 | 2021-04-27 | 杭州多能环保科技有限公司 | Preparation method of ion exchange resin for sulfolane purification |
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