CN105618164A - Regeneration method of decolorizing resin - Google Patents
Regeneration method of decolorizing resin Download PDFInfo
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- CN105618164A CN105618164A CN201610193197.4A CN201610193197A CN105618164A CN 105618164 A CN105618164 A CN 105618164A CN 201610193197 A CN201610193197 A CN 201610193197A CN 105618164 A CN105618164 A CN 105618164A
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Abstract
The invention discloses a regeneration method of decolorizing resin. The method comprises the following steps: firstly, cleaning a decolorizing resin column with fresh water with the volume being 1 to 2 times of that of the resin, then cleaning the decolorizing resin column with sodium hydroxide solution, pushing out liquid sodium hydroxide with compressed air, and then washing with water; secondly, leading in sodium chloride solution, soaking, then pushing out the sodium chloride solution with compressed air, repeating the process for 1 to 3 times, and finally washing with water. The invention further provides a recovery method of effluent brine during the regeneration process. The regeneration method can guarantee the regeneration effect of resin under the condition that the use level of sodium chloride is greatly reduced, greatly reduces the production cost, further reduces the discharge of brine, is environment-friendly, and has a very good industrial application prospect.
Description
Technical field
The present invention relates to the renovation process of a kind of decolorizing resin.
Background technology
Resin typically refers to softening or fusion range after being heated, have liquidity preference under external force, be solid-state, semi-solid state under normal temperature time softening, can also be liquid organic polymer sometimes. In a broad aspect, it is possible to any macromolecular compound processing raw material as plastics is all called resin. Decolorizing resin is generally macroporous ion exchange resin, owing to kind and purposes are all a lot, is widely used in food pharmaceutical industries such as the decolouring of Chinese herbal medicine effective ingredients decolouring, amino acid and alkaloids substance, Sugarcane juice decolorization, tartaric acid decolouring. Wherein chlorine type strong basic type anion-exchange resin is mainly with the decolouring of feed liquid in the production of antibiotics processes such as erythromycin.
For erythromycin production technique, various agricultural byproducts produce erythromycin and by product thereof through microorganism aerobic deep layer liquid state fermentation: a large amount of agricultural byproducts microbial cells residues etc. not being finished, above-mentioned feed liquid is first after the preliminary filtrations such as micro-filter, remove the above-mentioned residue of major part, again through decolorizing resin decolouring, then after nanofiltration system, enter downstream crystallisation workshop section. In its production process, resin needs constantly to regenerate, and in order to effective regeneration, current resin producer generally advises dynamic cleaning, namely first flow online cleaning with sodium hydroxide, the mode flowing with sodium-chlor and regenerating online again, this kind of mode needs to consume a large amount of sodium-chlor, had both needed a large amount of running cost, and had caused again environmental pollution.
At present, the mode solving this problem is reclaimed by sodium-chlor, minimizes cost, reduce environmental pollution, but due to cost recovery still very high, cause this process cost remain high. The sodium-chlor consumption reduced in decolorizing resin regenerative process is the basic way solving this problem, has no relevant at present and improves one's methods.
Summary of the invention
In order to solve the problem, the present invention provides the few resin regeneration method of a kind of sodium-chlor consumption.
The renovation process of chlorine type decolorizing resin of the present invention, comprises the steps:
(1) get pending decolorizing resin post, first by the clean water of resin 1-2 times of volume, then clean with sodium hydroxide solution, then with pressurized air, liquid sodium hydroxide is ejected, then rinse with water;
(2) add sodium chloride solution, soak, then eject sodium chloride solution with pressurized air, repeat 1-3 time, final rinse water.
Wherein eject sodium hydroxide solution or sodium chloride solution with pressurized air: refer to input compressed-air inside decolorizing resin post, until not having liquid to flow out.
Preferably, in step (1), described decolorizing resin be for the desolventing technology of the organic pigment in medicine and/or food and/or inorganic pigment after resin.
Preferably, described resin is chlorine type strong basic type anion-exchange resin.
Preferably, in step (1), the concentration of sodium hydroxide solution is 2.5-5.5%, it is preferable that 4%; And/or the volume of sodium hydroxide solution is 0.8-1.2 resin volume times, it is preferable to 1.0 times.
Preferably, in step (1), described water is tap water, primary reverse osmosis water or two-pass reverse osmosis water, it is preferable that primary reverse osmosis water; And/or, the consumption of described water is 0.8-1.2 times of resin volume, it is preferable to 1.0 times of resin volume.
Preferably, in step (1) and step (2), the pressure of pressurized air is 0.1 �� 0.05Mpa.
Preferably, in step (2), the sodium-chlor in described sodium chloride solution is refined salt or Industrial Salt; And/or, the concentration of described sodium chloride solution is 8-12%, it is preferable that 10%; And/or, the consumption of described sodium chloride solution is 0.8-1.2 times of resin volume, it is preferable to 1.0 times of resin volume; And/or, the number of times of described repetition is 2 times.
Preferably, in step (2), the time that sodium chloride solution soaks is 20-80min, it is preferable to 30min.
Preferably, step (2) described water is tap water, primary reverse osmosis water or two-pass reverse osmosis water, it is preferable that primary reverse osmosis water; And/or, the consumption of described water is 8-12 times of resin volume, it is preferable to 10 times of resin volume.
Present invention also offers the effluent brine recovery method in a kind of chlorine type decolorizing resin regenerative process, according to method described in aforementioned any one, chlorine type decolorizing resin is regenerated, in regenerative process, the waste water nanofiltration membrane molecular weight cut-off flowed out is the composition of 100-500 dalton, preferred molecular weight cut-off is the nanofiltration membrane of 250 dalton's compositions.
Renovation process of the present invention when greatly reducing sodium-chlor consumption, can ensure the regeneration effect of resin, considerably reduce production cost, decrease the discharge of salt solution, environmental friendliness, and prospects for commercial application is very good.
Below by embodiment, the present invention is described in further details, but it is not limitation of the present invention, foregoing according to the present invention, according to ordinary technical knowledge and the customary means of this area, do not departing under the above-mentioned basic fundamental thought prerequisite of the present invention, it is also possible to make the amendment of other various ways, replacement or change.
Accompanying drawing explanation
Fig. 1 regeneration and retrieving arrangement schematic diagram.
Embodiment
| Title material | Producer | Model |
| Resin | ROHM AND HAAS company of the U.S. | 98Cl, chlorine type strong base anion |
| Sodium hydroxide | Yi Li Nangang chemical industry limited liability company | Technical grade |
| Sodium-chlor (crude salt) | Yi Li salt industry limited liability company | Technical grade |
Experimental example 1 resin regeneration method of the present invention
1, renovation process
Get Yi Li Chuan Ning Bioisystech Co., Ltd and produce the decolorizing column (resin wherein is ROHM AND HAAS 98Cl, chlorine type strong base anion resins) in erythromycin process, regenerate as follows:
Get pending decolorizing column, as shown in Figure 1, first clean with the water of resin 1-2 times of volume, then from sodium hydroxide solution storage tank the sodium hydroxide solution that the concentration of 0.8 times of resin volume is 2.5% (g/g) is transported to decolorizing column with P2 pump and cleans, then the pressurized air being 0.1 �� 0.05Mpa with pressure ejects liquid caustic soda, then the water washing with 0.8 times of volume; Then it is 8% (g/g) sodium chloride solution be transported to decolorizing column static immersing displacement pigment from brine reservoir by the concentration of 0.8 times of resin volume with P3 pump, it is 20min every time, the pressurized air being all 0.1 �� 0.05Mpa with pressure after every time cleaning ejects sodium chloride solution, amount to 2 times, finally clean with the water of 8 times of resin volumes again.
Brine regeneration: the effluent brine every time produced, gets in effluent brine storage tank through P4 pump, then regenerates in P5 pump delivery to nanofiltration system, and the nanofiltration membrane molecular weight cut-off wherein regenerated is the composition of 100-500, it is preferable to 250. Salt solution after regeneration is sent in brine reservoir and is stored, and adds new Industrial Salt before the use so that it is working concentration reaches production requirement, i.e. 8-12% every time.
2, regenerated outcome
Detection method:
Get the destainer (in erythromycin production process) after decolouring by the decolorizing column after the decolorizing column before regeneration and regeneration respectively, detect its pH and transmittance. PH is directly with the desk-top pH meter detection of Mei Tele FE28, and transmittance detects under wavelength 500nm at domestic 721 type visible spectrophotometers.
Detected result is as shown in the table:
| Resin | Destainer PH value | Destainer transmittance |
| Before regeneration | 6.5 | 68% |
| After regeneration | 7.48 | 78.6% |
As can be seen from the above table, after adopting the inventive method to decolour, the pH of destainer improves, and transmittance significantly improves, illustrate the inventive method can residue in effective elimination resin, the regeneration effect of resin is excellent.
Experimental example 2 resin regeneration method of the present invention
1, renovation process
Get Yi Li Chuan Ning Bioisystech Co., Ltd and produce the decolorizing column (resin wherein is ROHM AND HAAS 98Cl, chlorine type strong base anion resins) in erythromycin process, regenerate as follows:
Get pending decolorizing column, as shown in Figure 1, first clean with the water of resin 1-2 times of volume, then from sodium hydroxide solution storage tank the sodium hydroxide solution that the concentration of 1.0 times of resin volumes is 4% (g/g) is transported to decolorizing column with P2 pump and cleans, then the pressurized air being 0.1 �� 0.05Mpa with pressure ejects liquid caustic soda, then the water washing with 1 times of volume; Then it is 10% (g/g) sodium chloride solution be transported to decolorizing column static immersing displacement pigment from brine reservoir by the concentration of 1.0 times of resin volumes with P3 pump, it is 30min every time, the pressurized air being all 0.1 �� 0.05Mpa with pressure after every time cleaning ejects sodium chloride solution, amount to 3 times, finally clean with the water of 10 times of resin volumes again.
Brine regeneration: the effluent brine every time produced, gets in effluent brine storage tank through P4 pump, then regenerates in P5 pump delivery to nanofiltration system, and the nanofiltration membrane molecular weight cut-off wherein regenerated is 100-500, it is preferable to 250. Salt solution after regeneration is sent in brine reservoir and is stored, and adds new Industrial Salt before the use so that it is working concentration reaches production requirement, i.e. 8-12% every time.
2, regenerated outcome
Detection method:
Get the destainer (in erythromycin production process) after decolouring by the decolorizing column after the decolorizing column before regeneration and regeneration respectively, detect its pH and transmittance. PH is directly with the desk-top ph meter detection of Mei Tele FE28, and transmittance detects under wavelength 500nm at domestic 721 type visible spectrophotometers.
Detected result is as shown in the table:
| Resin | Destainer PH value | Destainer transmittance |
| Before regeneration | 6.35 | 68.4% |
| After regeneration | 8.0 | 82.3% |
As can be seen from the above table, after adopting the inventive method to decolour, the pH of destainer improves, and transmittance significantly improves, illustrate the inventive method can residue in effective elimination resin, the regeneration effect of resin is excellent.
Experimental example 3 resin regeneration method of the present invention
1, renovation process
Get Yi Li Chuan Ning Bioisystech Co., Ltd and produce the decolorizing column (resin wherein is ROHM AND HAAS 98Cl, chlorine type strong base anion resins) in erythromycin process, regenerate as follows:
Get pending decolorizing column, as shown in Figure 1, first clean with the water of resin 1-2 times of volume, then from onium hydroxide solution sodium storage tank the sodium hydroxide solution that the concentration of 1.2 times of resin volumes is 5.5% (g/g) is transported to decolorizing column with P2 pump and cleans, then the pressurized air being 0.1 �� 0.05Mpa with pressure ejects liquid caustic soda, then the water washing with 1.2 times of volumes; Then it is 12% (g/g) sodium chloride solution be transported to decolorizing column static immersing displacement pigment from brine reservoir by the concentration of 1.2 times of resin volumes with P3 pump, it is 80min every time, the pressurized air being all 0.1 �� 0.05Mpa with pressure after every time cleaning ejects sodium chloride solution, amount to 4 times, finally clean with the water of 12 times of resin volumes again.
Brine regeneration: the effluent brine every time produced, gets in effluent brine storage tank through P4 pump, then regenerates in P5 pump delivery to nanofiltration system, and the nanofiltration membrane molecular weight cut-off wherein regenerated is 100-500, it is preferable to 250. Salt solution after regeneration is sent in brine reservoir and is stored, and adds new Industrial Salt before the use so that it is working concentration reaches production requirement, i.e. 8-12% every time.
2, regenerated outcome
Detection method:
Get the destainer (in erythromycin production process) after decolouring by the decolorizing column after the decolorizing column before regeneration and regeneration respectively, detect its pH and transmittance. PH is directly with the desk-top ph meter detection of Mei Tele FE28, and transmittance detects under wavelength 500nm at domestic 721 type visible spectrophotometers.
Detected result is as shown in the table:
| Resin | Destainer PH value | Destainer transmittance |
| Before regeneration | 6.87 | 68.8% |
| After regeneration | 8.0 | 78.6% |
As can be seen from the above table, after adopting the inventive method to decolour, the pH of destainer improves, and transmittance significantly improves, illustrate the inventive method can residue in effective elimination resin, the regeneration effect of resin is excellent.
The useful effect of the present invention is described by the mode of experimental example below:
In experimental example of the present invention, alkali lye and sodium hydroxide solution, salt solution and sodium chloride solution.
Experimental example 1
Get Yi Li Chuan Ning Bioisystech Co., Ltd and produce the decolorizing column (resin wherein is ROHM AND HAAS 98Cl, chlorine type strong base anion resins) in erythromycin process, regenerate as follows:
For erythromycin industrial production, get 600m3Upstream ceramic membrane (micro-filter) filtrate, it may also be useful to 5m3Decolorizing resin carry out desolventing technology, processing the decolorizing resin of filtrate, the mode first added with traditional stream is cleaned, and namely first cleans with the liquid caustic soda of 4% (g/g), eject liquid caustic soda with primary reverse osmosis water again, then prepare starting point concentration 9.94% (g/g) salt solution 20m3, flush time 2h, in detection effluent brine, sodium chloride concentration is 8.78%, it is seen that arriving of 20* (9.94-8.78) the % i.e. sodium-chlor of 0.232 ton of only having an appointment utilizes, and the salt of remaining 20*9.94%-0.232 that is 1.756 ton all discharges.
Get same decolorizing column again and process 600m equally3Filtrate, then carry out cleaning and regeneration by the method for the embodiment of the present invention 2, preparation starting point concentration 9.98% salt solution 15m3Leave standstill for three times and change regeneration, each 30min, finally detect salt concn in waste water and be respectively 7.56%, 8.62%, 9.22%, then effective salt consumption is 5* (3*9.88-7.56-8.62-9.22) %, namely 0.212 ton, the salt of remaining 15*9.88%-0.212 namely about 1.27 ton, above-mentioned salt is regenerated by nanofiltration system regeneration, efficiency 89.24%, then finally discharging salt total amount is 1.27*0.1076 that is 0.137 ton.
The two is more known, relative to existing purging method, it is few that the inventive method regenerates salt dosage every time, discharge salt amount less and it is about 2 tons, sodium-chlor uses saving rate to reach [20*9.94%-(0.212+0.137)/20*9.94%] * 100%, namely 82.44%, have huge economic worth and environment protection significance.
Experimental example 2
Experimental technique kind, except brine concentration is adjusted to 10.01% (g/g) salt solution, all the other are with experimental example 1.
Adopting existing method to regenerate, in detection waste water, salt concn is 8.74%, then salt utilization and output are respectively 0.254 ton and 1.748 tons.
Again with the inventive method regeneration, in detection waste water, salt concn is 7.80%, 8.92%, 9.16%, then salt utilization and output are respectively 0.211 ton and 1.291 tons, then carry out salt Water Sproading, then finally discharging salt total amount is 0.1389 ton.
The two being compared it will be seen that relative to existing purging method, it is few that the inventive method regenerates salt dosage every time, sodium-chlor uses saving rate to reach [20*10.01%-(0.211+0.1389)/20*10.01%] * 100%, is 82.52%.
Experimental example 3
The regeneration of decolorizing resin is carried out, to produce the amount that ton Matachrom calculates the annual sodium-chlor saved per year according to the patent of type of the present invention:
Production level domestic at present is every ton of erythromycin fermentation liquid, can produce about 8kg Matachrom, and every ton of erythromycin fermentation liquid arrives decolouring post through pre-treatment above, and quality is increased to about 2.5 tons, and a loading amount is 5m3Decolorizing column can disposable maximum decolouring 600 cubic metres (about 600 tons), be then 2 tons by sodium-chlor quality when regenerating. It is 1.0417 tons that finally calculating production one ton of Matachrom needs to spend sodium-chlor amount, then producing ten thousand tons of Matachroms then needs to consume 10417 tons of sodium-chlor/years, adopts the method for this patent then can save 9300 tons of sodium-chlor/years.
Calculate known, the preparation of Matachrom adopt the inventive method to regenerate, 9300 tons of sodium-chlor/years can be saved, directly saving Financial cost is 7,440,000 yuan/ten thousand tons Matachroms (industry sodium-chlor is according to 800 yuan/ton), achieve commercial success, and be equivalent to few discharge pure sodium chloride about 9300 tons every year, make huge contribution to domestic environmental protection cause.
To sum up, renovation process of the present invention can residue in effective elimination resin, the regeneration effect of resin is excellent, and salt dosage is significantly less than existing renovation process less, economic benefit clearly, achieves commercial success, and sodium-chlor discharge is few, environmental friendliness, prospects for commercial application is very excellent.
Claims (10)
1. the renovation process of a decolorizing resin, it is characterised in that: comprise the steps:
(1) get pending decolorizing resin post, first by the clean water of resin 1-2 times of volume, then clean with sodium hydroxide solution, then with pressurized air, liquid sodium hydroxide is ejected, then rinse with water;
(2) add sodium chloride solution, soak, then eject sodium chloride solution with pressurized air, repeat 1-3 time, final rinse water.
2. renovation process according to claim 1, it is characterised in that: in step (1), described decolorizing resin be for the desolventing technology of the organic pigment in medicine and/or food and/or inorganic pigment after resin.
3. generation method according to claim 1 and 2, it is characterised in that: described resin is chlorine type strong basic type anion-exchange resin.
4. renovation process according to claim 1, it is characterised in that: in step (1), the concentration of sodium hydroxide solution is 2.5-5.5%, it is preferable that 4%; And/or the volume of sodium hydroxide solution is 0.8-1.2 resin volume times, it is preferable to 1.0 times.
5. renovation process according to claim 1, it is characterised in that: in step (1), described water is tap water, primary reverse osmosis water or two-pass reverse osmosis water, it is preferable that primary reverse osmosis water; And/or, the consumption of described water is 0.8-1.2 times of resin volume, it is preferable to 1.0 times of resin volume.
6. renovation process according to claim 1, it is characterised in that: in step (1) and step (2), the pressure of pressurized air is 0.1 �� 0.05Mpa.
7. renovation process according to claim 1, it is characterised in that: in step (2), the sodium-chlor in described sodium chloride solution is refined salt or Industrial Salt; And/or, the concentration of described sodium chloride solution is 8-12%, it is preferable that 10%; And/or, the consumption of described sodium chloride solution is 0.8-1.2 times of resin volume, it is preferable to 1.0 times of resin volume; And/or, the number of times of described repetition is 2 times.
8. renovation process according to claim 1, it is characterised in that: in step (2), the time that sodium chloride solution soaks is 20-80min, it is preferable to 30min.
9. renovation process according to claim 1, it is characterised in that: step (2) described water is tap water, primary reverse osmosis water or two-pass reverse osmosis water, it is preferable that primary reverse osmosis water; And/or, the consumption of described water is 8-12 times of resin volume, it is preferable to 10 times of resin volume.
10. the effluent brine recovery method in a chlorine type decolorizing resin regenerative process, it is characterized in that: according to method described in claim 1-9 any one, chlorine type decolorizing resin is regenerated, in regenerative process, the waste water nanofiltration membrane molecular weight cut-off flowed out is the composition of 100-500 dalton, preferred molecular weight cut-off is the nanofiltration membrane of 250 dalton's compositions.
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Cited By (7)
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| CN106732832A (en) * | 2017-01-23 | 2017-05-31 | 湖南农业大学 | The method for reclaiming EDTA metal complexs and regeneration Chioro-anion exchange resin using metal salt solution |
| CN107840412A (en) * | 2017-12-11 | 2018-03-27 | 淄博格瑞水处理工程有限公司 | A kind of zero-emission softened water equipment |
| CN110062657A (en) * | 2016-11-24 | 2019-07-26 | 诺瓦塞普工艺公司 | Use the purification process of low granularity resin |
| CN111068634A (en) * | 2019-12-27 | 2020-04-28 | 四川省玉鑫药业有限公司 | Regeneration method of alumina column |
| CN111905842A (en) * | 2020-08-21 | 2020-11-10 | 四川省宜宾惠美线业有限责任公司 | Method for treating poisoned anion resin |
| CN112410474A (en) * | 2020-11-16 | 2021-02-26 | 南京甘汁园糖业有限公司 | Ion exchange decoloration water-saving process for refined sugar |
| CN114522744A (en) * | 2022-01-24 | 2022-05-24 | 信丰华锐钨钼新材料有限公司 | Method for washing, desorbing and regenerating D363 resin |
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| CN110062657A (en) * | 2016-11-24 | 2019-07-26 | 诺瓦塞普工艺公司 | Use the purification process of low granularity resin |
| CN106732832A (en) * | 2017-01-23 | 2017-05-31 | 湖南农业大学 | The method for reclaiming EDTA metal complexs and regeneration Chioro-anion exchange resin using metal salt solution |
| CN106732832B (en) * | 2017-01-23 | 2019-05-10 | 湖南农业大学 | EDTA metal complex is recycled using metal salt solution and regenerates the method for Chioro-anion exchange resin |
| CN107840412A (en) * | 2017-12-11 | 2018-03-27 | 淄博格瑞水处理工程有限公司 | A kind of zero-emission softened water equipment |
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| CN111068634A (en) * | 2019-12-27 | 2020-04-28 | 四川省玉鑫药业有限公司 | Regeneration method of alumina column |
| CN111068634B (en) * | 2019-12-27 | 2022-07-08 | 四川省玉鑫药业有限公司 | Regeneration method of alumina column |
| CN111905842A (en) * | 2020-08-21 | 2020-11-10 | 四川省宜宾惠美线业有限责任公司 | Method for treating poisoned anion resin |
| CN112410474A (en) * | 2020-11-16 | 2021-02-26 | 南京甘汁园糖业有限公司 | Ion exchange decoloration water-saving process for refined sugar |
| CN112410474B (en) * | 2020-11-16 | 2023-09-15 | 南京甘汁园股份有限公司 | Ion exchange decoloring water-saving process for refining sugar |
| CN114522744A (en) * | 2022-01-24 | 2022-05-24 | 信丰华锐钨钼新材料有限公司 | Method for washing, desorbing and regenerating D363 resin |
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