CN104483397A - An evaluating method for resin adsorption performance in a phenol refining process - Google Patents
An evaluating method for resin adsorption performance in a phenol refining process Download PDFInfo
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- CN104483397A CN104483397A CN201410544776.XA CN201410544776A CN104483397A CN 104483397 A CN104483397 A CN 104483397A CN 201410544776 A CN201410544776 A CN 201410544776A CN 104483397 A CN104483397 A CN 104483397A
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Abstract
The invention belongs to the technical field of resin evaluation, and mainly relates to an evaluating method for resins in a phenol refining process. The evaluating method mainly relates to evaluation of adsorption performance of two resins. Firstly, the total ion-exchange capacity of each resin is measured, and then the adsorption performance of each of the resins is evaluated by utilization of static adsorption and dynamic adsorption methods. A method combining headspace solid-phase microextraction and gas chromatography is utilized for measuring impurity contents in phenol in the whole evaluating process. The evaluating method is simple in operation and comprehensive in applications, can be used for evaluation of all resins in industrial applications, and has a good using prospect in the field of fine chemicals.
Description
Technical field
The invention belongs to resin assessment technique field, mainly relate in phenol extraction process the method that resin is evaluated.
Background technology
Phenol, has another name called carbolic acid, is basic organic important in chemical production, is widely used in synthon, phenolics, the every field such as medicine and agricultural chemicals.At present, what global phenol had 90 more than ﹪ to adopt is that production phenols synthesizes, and the method is easy to operate, and output is higher, simultaneously can cogeneration of propanone.But in process of production, the method produces the organic impurities of multiple more difficult removing, seriously have impact on purity and the color and luster of phenol, bring many difficulties also can to follow-up production, directly can affect the value of phenol product.
Phenol is exquisite resin dedicated is that the organic impurities research and development be used for specially in adsorbing phenol production run form, and the basic framework that this resinoid is is resin with poly-divinylbenzene is ion-exchange group with sulfonic group, generates a kind of highly acid ion exchange resin.
Current, to the evaluation method of resin mainly to the research of its absorption property, but research just rests on the performance of part, its research is not formed to the method for system.Main each performance from resin is systematically studied it herein, and research method is simple to operate, and Instrument Design application is convenient, and has good reference to resin evaluation.
Summary of the invention
The object of the present invention is to provide the method for evaluating resin performance in a set of Pyrogentisinic Acid's delicate procedure, the total ion exchange capacity that this method is mainly concerned with resin measures, Static Adsorption and Dynamic Adsorption three aspects, and wherein the assay method of total ion exchange capacity is:
(1) blank assay: pipette 20 ml NaOH titers with transfer pipet, be placed in conical flask, add 30 ml distilled water and 3 dimethyl diaminophenazine chloride indicator, now conical flask is in golden yellow, with HCl titer be titrated to solution become pale red and keep 15 s colour-fast till, recording volume V
2.
(2) exchange capacity measures: on analytical balance, take each 1.50 g of pretreated two kinds of resins, often kind of resin takes three parts, be placed in dry conical flask respectively, in each conical flask, NaOH titer 100 ml is added with transfer pipet, fully shake up sealing, soak 4 h at normal temperatures.Upper strata soak solution 20 ml is always pipetted from conical flask, be placed in another conical flask, add 30 ml distilled water and 3 dimethyl diaminophenazine chloride indicator wherein, the solution now in conical flask presents golden yellow, to be titrated in pale red with hydrochloric acid standard solution and till keeping 15 s colour-fast, recording volume V
1.
Following formula is utilized to calculate the exchange capacity of resin
Formula:
Q in formula
t-Zeo-karb butt CEC, mmolg
-1; C
hClthe concentration of-hydrochloric acid standard solution, molL
-1; V
2-blank assay consumes the volume of hydrochloric acid standard solution, ml; V
1-titration resin soaks the volume of the hydrochloric acid standard solution that supernatant liquor consumes, ml; M
1the quality of-resin sample, g.
The evaluation method of Static Adsorption is:
Weighing quantity of resin and liquid crude phenol put into conical flask with different mass ratioes, bottleneck is sealed with preservative film, conical flask is put into constant temperature oscillator and shake 4 h, temperature controls at 60 DEG C-65 DEG C, take out appropriate phenol after concussion to put into sample bottle and carry out solid-phase microextraction, subsequently solid-phase micro-extracting device is resolved in gas chromatography, utilize area normalization method to obtain peak area, recorded the content of impurity by working curve.
The evaluation method of Dynamic Adsorption is:
Fill the resin of 4.0 cm-20 about cm height in glass column, add appropriate liquid crude phenol in separating funnel, first phenol is heated to be in a liquid state before experiment, regulate with cock and with certain flow velocity, phenol is flowed in glass column.Glass column entrance and glass column all will take insulation, and glass column external application heating tape is wound around, and utilizes pressure regulation temperature controller control temperature, general pressure is when 150 V, can ensure that in post, temperature is between 70 DEG C-85 DEG C, phenol in post can not be solidified, and resin normally adsorbs.Glass column outlet utilizes cock to regulate flow velocity, and ensures phenol liquid level constant in post.Discharge hose is wound around with heating tape, with Anti-solidification equally.Use the beaker of 200 ml to receive phenol, collect the sample of certain volume.Collect phenol with sample bottle and be used for analytical test, with concentration ratio (instant concentration C/initial concentration C
0) evaluate the change of impurity content.Carry out the absorption property of evaluating resin with penetration volume (during resin complete deactivation, phenol flows through the volume of resin bed), Dynamic Adsorption curve Logestic equation carries out matching, finds out adsorption curve flex point, i.e. penetration volume.
Accompanying drawing explanation
Fig. 1 is 2-methyl benzofuran comparison diagram in two kinds of resin Static Adsorption phenol
Fig. 2 is designed, designed dynamic adsorption test installation drawing.
Wherein 1 resin bed, 2 inner layer glass sleeve pipes, 3 glass outer sleeve pipes, the separating funnel skin of 4 splendid attire phenol has Resistant heating
Fig. 3 is 2-methyl benzofuran comparison diagram in two kinds of resin Dynamic Adsorption phenol
Embodiment
Exchange capacity measures example:
After blank test, analytical balance takes pretreated KC113 resin and each 1.50 g of import resin, and often kind of resin takes three parts, be placed in dry conical flask respectively, in each conical flask, add NaOH titer 100 ml with transfer pipet, fully shake up sealing, soak 4 h at normal temperatures.Upper strata soak solution 20 ml is always pipetted from conical flask, be placed in another conical flask, add 30 ml distilled water and 3 dimethyl diaminophenazine chloride indicator wherein, solution now in conical flask presents golden yellow, be that 0.12 mol/L hydrochloric acid standard solution is titrated in pale red and till keeping 15 s colour-fast, records volume V by concentration
1.
Table 1 blank assay data
V
2=V
stop-V
initially
Table 2 exchange capacity measures
Static Adsorptive capacity measures example:
Take crude phenol respectively and be respectively 1.5:1,2:1,2.5:1,3:1 with KC113 and import resin quality ratio, 3.5:1,4:1 sample, stirs 30min by it at 60 DEG C, get in about 0.1g phenol sample and solid-phase microextraction sample bottle, add 400uL methyl alcohol and 4mL water, ultrasonic vibration is to clarification.Control optimal conditions to extract, after extraction, carry out Thermal desorption to gas chromatographic sample introduction mouth, chromatogram is analyzed, utilize area normalization method to obtain peak area value.
Dynamic adsorption measures example:
KC113 and import resin 5 cm of same resin bed height is added respectively in resin bed, control phenol flow velocity is identical is 1.0 mL/min, the phenol that this different time flows out is tested, record flowed out the volume of phenol at that time, and using the volume of outflow as horizontal ordinate, concentration ratio (instant concentration/initial concentration) makes ordinate, draw elution curve, utilize Logestic equation to carry out matching, the curve after matching is drawn, contrasts.
Claims (6)
1. a set of method for evaluating resin adsorption performance in phenol delicate procedure, it is characterized in that: to the summary of the evaluation method of resin, respectively from the ion-exchange total volume of resin, Static Adsorptive capacity, comprehensive evaluation is carried out with dynamic adsorption, and whole evaluation procedure utilizes the method for solid-phase microextraction and gas chromatography coupling to measure its content, and concrete evaluation method is as follows:
(1) resin is carried out pre-service, process post-drying is for subsequent use;
(2) take each 1.5 g of resin respectively, three parts often kind, measure its ion-exchange total volume;
(3) weighing quantity of resin and phenol solution put into conical flask with different mass ratioes, bottleneck is sealed with preservative film, conical flask is put into constant temperature oscillator and shake 4 h, temperature controls at 60 DEG C-65 DEG C, take out about 0.1 g phenol sample after concussion and carry out solid-phase microextraction in sample bottle, find out the optimum quality ratio of Static Adsorption resin and phenol;
(4) fill the resin of 4.0 cm-20 about cm height in glass column, add appropriate liquid crude phenol in separating funnel, first phenol is heated to be in a liquid state before experiment, regulate with cock and with certain flow velocity, phenol is flowed in glass resin bed.
2. utilize pressure regulation temperature controller control temperature, general pressure, when 150 V, can ensure that in post, temperature is between 70 DEG C-85 DEG C, and phenol in post can not be solidified, and resin normally adsorbs.
3. a set of method for evaluating resin adsorption performance in phenol delicate procedure according to claim 1, is characterized in that, carries out systematic research to the ion exchange capacity of resin.
4. a set of method for evaluating resin adsorption performance in phenol delicate procedure according to claim 1, it is characterized in that, shake 4 h during Static Adsorption in process in constant temperature oscillator, and temperature controls at 60 DEG C-65 DEG C.
5. a set of method for evaluating resin adsorption performance in phenol delicate procedure according to claim 1, is characterized in that, utilize the method for solid-phase microextraction and gas chromatography coupling to measure impurity content and change.
6. a set of method for evaluating resin adsorption performance in phenol delicate procedure according to claim 1, it is characterized in that, the device used in Dynamic Adsorption process is the device of designed, designed, and resin bed potting resin height is 4.0 cm-20 cm, Control of Voltage is at 150 V, and temperature controls at 70 DEG C-85 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105929064A (en) * | 2016-04-25 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for determining residual quantity of organic solvent in terpene resin by using ASE-HPLC |
| CN112198274A (en) * | 2020-11-02 | 2021-01-08 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
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| JP2002048776A (en) * | 2000-08-07 | 2002-02-15 | Japan Organo Co Ltd | Performance evaluation method and device of anion- exchange resin and condensate demineralizer |
| CN1668917A (en) * | 2002-07-11 | 2005-09-14 | 奥甘诺株式会社 | Method for evaluating cation-exchage resin and method for controlling water treatment system using the same |
| CN101984343A (en) * | 2010-10-22 | 2011-03-09 | 浙江大学 | Method of discriminating key points in macroporous resin separation and purification process of traditional Chinese medicines |
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| JP2002048776A (en) * | 2000-08-07 | 2002-02-15 | Japan Organo Co Ltd | Performance evaluation method and device of anion- exchange resin and condensate demineralizer |
| CN1668917A (en) * | 2002-07-11 | 2005-09-14 | 奥甘诺株式会社 | Method for evaluating cation-exchage resin and method for controlling water treatment system using the same |
| CN101984343A (en) * | 2010-10-22 | 2011-03-09 | 浙江大学 | Method of discriminating key points in macroporous resin separation and purification process of traditional Chinese medicines |
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| 娄大伟 等: "固相微萃取-气相色谱法测定工业苯酚中的2-甲基苯并呋喃和2 , 4-二苯基-4-甲基-1-戊烯", 《色谱》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105929064A (en) * | 2016-04-25 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for determining residual quantity of organic solvent in terpene resin by using ASE-HPLC |
| CN112198274A (en) * | 2020-11-02 | 2021-01-08 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
| CN112198274B (en) * | 2020-11-02 | 2022-04-05 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
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Application publication date: 20150401 |