EP0150023A2 - Procédé pour le nettoyage d'un liquide de mercérisation - Google Patents
Procédé pour le nettoyage d'un liquide de mercérisation Download PDFInfo
- Publication number
- EP0150023A2 EP0150023A2 EP85100263A EP85100263A EP0150023A2 EP 0150023 A2 EP0150023 A2 EP 0150023A2 EP 85100263 A EP85100263 A EP 85100263A EP 85100263 A EP85100263 A EP 85100263A EP 0150023 A2 EP0150023 A2 EP 0150023A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- flotation
- mercerizing
- liquor
- lye
- naoh
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title abstract description 15
- 238000000746 purification Methods 0.000 title description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 61
- 238000005188 flotation Methods 0.000 claims abstract description 31
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000005517 mercerization Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 description 12
- 239000000356 contaminant Substances 0.000 description 10
- 239000006260 foam Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000004061 bleaching Methods 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 230000015271 coagulation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000004071 soot Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- -1 peroxide compounds Chemical class 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000984 vat dye Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- FMWAXKQEIXRUTI-UHFFFAOYSA-N dodecyl hydrogen sulfate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(O)(=O)=O FMWAXKQEIXRUTI-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 229910003439 heavy metal oxide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
Definitions
- the invention relates to a process for the purification of a least 20 g / l NaOH containing mercerization particularly solid impurities, wherein an addition of at least O, 1 vol .-% to 30% H 2 0 2 corresponding quantity of H 2 O 2 added to the mercerizing liquor and the impurities are separated off by flotation.
- CH-A-604 815 describes such a process, which is aimed at soot particles, which were formed by burning away free-standing fibers before the mercerization and which got into the liquor during the mercerization, either to oxidize or to coagulate to such an extent that they from the Lye can be separated.
- the decomposition of H 2 0 2 is catalyzed with manganese dioxide, since both the oxidation and the coagulation depend on a sufficient supply of nascent oxygen.
- the coagulated particles are separated in a separate process step, the flotation being mentioned as the separation method.
- finely dispersed soot particles are by no means the first of the contaminants that have to be removed from a used mercerizing liquor, in particular the problem of soot dust does not arise at all if the cotton is not seared before mercerizing.
- a process for cleaning mercerizing lye will find a wide range of applications, especially if it is possible to remove not only fibers and dispersed dirt particles, but above all dyes, especially vat dyes, from the lye.
- CH-PS 604 815 In contrast to the situation on which CH-PS 604 815 is based, it is generally not the lack of coagulation of finely dispersed particles that is the problem which prevents the efficient cleaning of mercerizing liquors, but rather the lack of simple and inexpensive separation processes, especially flotation processes. Even if the coagulation of the impurities obtained according to the prior art should make it possible to separate them by simple filtration, the known method has the disadvantage that the heavy metal oxide used in a later peroxide bleaching, which in itself is the preferred bleaching method, acts as a bleaching poison and is also a cost factor.
- the invention is based on the surprising finding that, even without the use of catalysts and thus the rapid decomposition of H 2 0 2 , which is the basis of the process according to CH-A-604 815, it is possible to purify mercerizing solutions by means of H 2 0 2 is. In this case, however, the cleaning effect is based primarily on the chemical flotation which the oxygen released during H 2 0 2 decomposition brings about. It is known in principle that the gas bubbles on which every flotation process is based can be generated using peroxide compounds, but was still referred to in 1969 (cf. Reinhold Köhler in "Water, Air and Operation", page 324) as only of theoretical interest.
- the invention is therefore based on the object of modifying a method of the type outlined in CH-A-604 815 such that on the one hand the use of bleaching poisons can be dispensed with and on the other hand an additional separation process is unnecessary. This is achieved in that the mixture of mercerizing liquor and H 2 ⁇ 2 is kept essentially free of heavy metal catalysts and allowed to stand for at least 15 minutes so that the oxygen released upon decomposition of the H 2 O 2 causes the flotation.
- the density of the treated lye is only critical for the process insofar as the decomposition of the H 2 O 2 without catalysts only takes place sufficiently quickly in the sufficiently basic range, for example from a pH of 13.7.
- the mercerizing solution is obtained anyway with a concentration of 40 g / 1, which corresponds to a pH value of 14.
- it is now advantageous to thicken the alkali since evaporation of the alkali is cheaper than using large amounts of H 2 O 2 .
- the thickening of the alkali also has the advantage that the contaminants float more easily, whereas an excessively thick alkali hinders the floating due to its high viscosity.
- Usual cleaning methods such as centrifugation, filtration, compressed air flotation or electroflotation, are inferior to the described method, especially with higher viscosities.
- the optimal value of the concentration is 300g / 1 or - more often - between 400 and 420 g / 1, depending on the type of the main impurities.
- the influence of temperature on the process is comparable to that of the H 2 O 2 concentration: if the temperature is increased, the HzOz decomposes more quickly. However, this leads to turbulence in the liquid and a poorer degree of cleaning.
- the temperature will therefore be chosen high enough not to lead to unreasonably long treatment times, but on the other hand not higher than necessary in order not to deteriorate the result of the process. Temperatures in the range between 20 ° C and 40 ° C have proven to be favorable in most cases. In the case of various crude mercerization liquors, it has proven advantageous to heat the liquor to temperatures of up to 80 ° C., preferably 40-60 ° C. for 10 minutes and then to allow it to cool to room temperature within 1-2 hours. The flotation of the contaminants occurs especially during the cooling phase.
- a Mischbe container 3 which contains a mixer 6, unpurified lye from container 2 and H 2 0 2 from container 1 mixed.
- the mixing time should not exceed 30 minutes, preferably 15 minutes, particularly advantageously 5 minutes. Otherwise the H 2 0 2 decomposition already begins to a noticeable extent.
- the mixing temperature is advantageously set between 15 ° and 30 ° C. Higher temperatures up to 90 ° C can also be used.
- the mixing time should then be as short as possible. Instead of a 30% HzOz solution, an appropriately diluted solution can be used for easier dosing.
- the mixture is passed into the flotation tank 4. A speed control of the flotation is possible by setting a certain temperature of the lye.
- the caustic solution itself could be heated before the HzGz admixture, between the mixing container 3 and the flotation container 4 or in the flotation container 4.
- the mixture is passed through a heat exchanger 5 for this purpose, which can work in a known manner according to the countercurrent principle.
- the device shown can be operated continuously or in batches. Valves 7 - 14 and peristaltic pumps 15 - 18 are used to control the process.
- a flocculation of the alkali contaminants and above all a flotation of the undissolved contaminants takes place in the flotation container 4.
- dissolved colored compounds are also bleached, so that cleaning does not only take place with regard to the dispersed contaminants.
- an oxidizing flotation agent is particularly advantageous for the removal of vat dyes, since these become water-insoluble as a result of oxidation and are thus completely removed by flotation. Especially It is noteworthy that the flotation process is also able to accumulate certain dissolved compounds, such as starch, polyethylene glycols, fatty acids, in the foam layer. It is therefore not only possible to remove oxidatively but also to remove dissolved contaminants.
- the foam layer formed during the flotation of mercerizing liquors or evaporated mercerizing liquors is sufficiently stable to be removed by conventional methods for separating flotation foams.
- the removal is carried out by sucking air through the pump 19 and valves 9 and 12, whereby the foam is deposited in the container 20.
- the pure liquor is pumped into the container 21 by means of the hose pump 18 via the valve 10, a remaining sediment reaches the container 22 under the influence of the vacuum pump 19 via the valve 11.
- the equipment required for the device shown is low compared to electroflotation for lye cleaning. Compared to pressure relaxation flotation, chemical gas bubble generation according to the invention leads to incomparably higher amounts of gas available.
- a mercerizing liquor concentrated by evaporation was used as the unpurified lye.
- the liquor contained 402 g / l NaOH and 37.5 g / 1 Na 2 CO 3 .
- 50 ml of alkali were vigorously mixed with 0.5 ml and 13% H 2 O 2 for one minute at 20 ° C.
- the mixture was slowly warmed to 30 ° C in a water bath without stirring.
- the course of the boundary between foam and purified lye is shown in Table 1.
- the foam layer was removed by suction.
- the cleaning effect was assessed by determining the COD value (chemical oxygen requirement for the breakdown of the impurities to CO 2 and water).
- the dispersed impurities were removed, the remaining COD was caused by dissolved impurities.
- the lye was cleaned in a continuously operating apparatus, as shown in the drawing. H 2 O 2 and NaOH were fed into the mixing tank by a metering pump containers were conveyed from there to the flotation tank (volume approx. 2 1). The cleaned lye was continuously removed from the container.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Paper (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT0016284A AT392097B (de) | 1984-01-19 | 1984-01-19 | Verfahren zur reinigung von mercerisierlauge |
AT162/84 | 1984-01-19 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0150023A2 true EP0150023A2 (fr) | 1985-07-31 |
EP0150023A3 EP0150023A3 (en) | 1986-02-12 |
EP0150023B1 EP0150023B1 (fr) | 1988-12-21 |
Family
ID=3483199
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP19850100263 Expired EP0150023B1 (fr) | 1984-01-19 | 1985-01-12 | Procédé pour le nettoyage d'un liquide de mercérisation |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0150023B1 (fr) |
AT (1) | AT392097B (fr) |
DE (1) | DE3566914D1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5837977A (en) * | 1995-06-07 | 1998-11-17 | Quiclave, L.L.C. | Microwave heating container with microwave reflective dummy load |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111847626B (zh) * | 2020-07-27 | 2022-08-05 | 南昌航空大学 | 一种利用催化氧化法对电镀清洗废水中络合态重金属进行预处理的装置的使用方法 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2521157A1 (de) * | 1975-05-13 | 1976-11-25 | Ags Ausruestungsgesellschaft F | Verfahren und vorrichtung zur reinigung von mercerisierlauge |
DE2641094A1 (de) * | 1976-08-24 | 1978-03-02 | Bbc Brown Boveri & Cie | Verfahren zur reinigung einer alkalischen loesung und einrichtung zur durchfuehrung des verfahrens |
-
1984
- 1984-01-19 AT AT0016284A patent/AT392097B/de not_active IP Right Cessation
-
1985
- 1985-01-12 DE DE8585100263T patent/DE3566914D1/de not_active Expired
- 1985-01-12 EP EP19850100263 patent/EP0150023B1/fr not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2521157A1 (de) * | 1975-05-13 | 1976-11-25 | Ags Ausruestungsgesellschaft F | Verfahren und vorrichtung zur reinigung von mercerisierlauge |
DE2641094A1 (de) * | 1976-08-24 | 1978-03-02 | Bbc Brown Boveri & Cie | Verfahren zur reinigung einer alkalischen loesung und einrichtung zur durchfuehrung des verfahrens |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5837977A (en) * | 1995-06-07 | 1998-11-17 | Quiclave, L.L.C. | Microwave heating container with microwave reflective dummy load |
Also Published As
Publication number | Publication date |
---|---|
ATA16284A (de) | 1985-08-15 |
DE3566914D1 (en) | 1989-01-26 |
EP0150023B1 (fr) | 1988-12-21 |
EP0150023A3 (en) | 1986-02-12 |
AT392097B (de) | 1991-01-25 |
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