CN103467275A - Catalytic oxidation production method of sodium gluconate liquid by means of activated carbon treatment - Google Patents
Catalytic oxidation production method of sodium gluconate liquid by means of activated carbon treatment Download PDFInfo
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- CN103467275A CN103467275A CN2013104200036A CN201310420003A CN103467275A CN 103467275 A CN103467275 A CN 103467275A CN 2013104200036 A CN2013104200036 A CN 2013104200036A CN 201310420003 A CN201310420003 A CN 201310420003A CN 103467275 A CN103467275 A CN 103467275A
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- gac
- mixing solutions
- sodium gluconate
- activated carbon
- solution
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- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229940005574 sodium gluconate Drugs 0.000 title claims abstract description 40
- 235000012207 sodium gluconate Nutrition 0.000 title claims abstract description 40
- 239000000176 sodium gluconate Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 230000003647 oxidation Effects 0.000 title claims abstract description 33
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 33
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 title abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000007667 floating Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- 239000003610 charcoal Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 6
- 210000003298 dental enamel Anatomy 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 239000006210 lotion Substances 0.000 claims description 6
- 238000011085 pressure filtration Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 6
- 235000020679 tap water Nutrition 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 27
- 229910052797 bismuth Inorganic materials 0.000 abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052763 palladium Inorganic materials 0.000 abstract description 10
- 238000011010 flushing procedure Methods 0.000 abstract 2
- 238000009835 boiling Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Water Treatment By Sorption (AREA)
Abstract
The invention relates to a catalytic oxidation production method of a sodium gluconate liquid by means of activated carbon treatment, which can effectively solve and prevent the problems of palladium loss and bismuth loss in the catalytic oxidation production process of the sodium gluconate liquid. The catalytic oxidation production method comprises the following steps: the treatment of the activated carbon: soaking the activated carbon in deionized water, causing the resulting product to stand still, and removing the floating dredge on the upper layer; adding the soaked activated carbon and water into a reactor for uniform mixing to obtain an activated carbon mixed liquid, adding nitric acid into the activated carbon mixed liquid, boiling the resulting liquid for 4-5 hours and reducing the temperature of the liquid; separating the activated carbon from the mixed liquid, and slowly flushing the separated activated carbon using the deionized water until the conductivity of the discharged flushing liquid is not more than 50mu s/cm; and the treatment of the sodium gluconate liquid: adding the sodium gluconate oxidizing liquid into the treated activated carbon, starting the mixing, heating the resulting product to 70-80 DEG C, preserving the temperature for 0.5-3.0h, and filtering the resulting product under pressure to obtain the clear and transparent sodium gluconate liquid and the activated carbon. The method provided by the invention is simple, easy to operate, small in palladium loss and bismuth loss, capable of saving resources, and is an innovation in the production of the sodium gluconate.
Description
Technical field
The present invention relates to chemical industry, particularly a kind of method of the sodium gluconate solution of producing with the activated carbon treatment catalytic oxidation.
Background technology
When catalytic oxidation is produced sodium gluconate solution, use be the Pd(palladium)-the Bi(bismuth)-C(carbon) catalyzer.In the process of producing because use equipment is cyclic spray formula stills for air blowing, the carrier active carbon of catalyzer is broken serious, cause active component palladium (Pd), the bismuth (Bi) of catalyzer to drop in sodium gluconate solution, cause the sodium gluconate solution heavy metal content to exceed standard, and palladium (Pd), bismuth (Bi) loss are seriously, and the rate of loss of palladium (Pd) reaches 35% by statistics, and the rate of loss of bismuth (Bi) reaches 45%, both cause raw-material waste, caused again the increase of product cost.Therefore how solving the loss that prevents palladium, bismuth when catalytic oxidation is produced sodium gluconate solution, is technical problem urgently to be resolved hurrily.
Summary of the invention
For the problems referred to above, for overcoming the defect of prior art, the present invention's purpose just is to provide a kind of method of the sodium gluconate solution of producing with the activated carbon treatment catalytic oxidation, can effectively solve the loss problem that prevents palladium, bismuth when catalytic oxidation is produced sodium gluconate solution.
The technical scheme that the present invention solves is to comprise the following steps:
One, the processing of gac:
(1), bubble charcoal: method is gac to be soaked to standing 1.5-2.0h with deionized water, abandon its upper strata floating matter, so repeatedly, (eliminating floating matter) no longer occur to the upper strata floating matter, then gac is separated from solution, obtained brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio 1: 3(, be solid-to-liquid ratio 1: 3) join in enamel reactor, stir, become the gac mixing solutions, add again the nitric acid of mass concentration 65%-68% in the gac mixing solutions, the 1-2.0% that the nitric acid add-on is gac mixing solutions weight, slowly heat to 100 ℃-110 ℃, boil 4-5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is separated, gac is separated from mixing solutions, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm with deionized water, continue to separate 0.5-1.0h, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is that the gac that adds Sunmorl N 60S oxidation solution weight 1%-2% step 1 to process the Sunmorl N 60S oxidation solution, open and stir, and is heated to 70-80 ℃, is incubated 0.5-3.0h, obtains mixing solutions;
(2), pressure filtration: mixing solutions is filtered under the pressure of 0.1-0.15Mpa, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, and gac can reuse.
The inventive method is simple, easy to operate, and the loss amount of palladium, bismuth is little, economizes on resources, and is the innovation during Sunmorl N 60S is produced.
Embodiment
Below in conjunction with particular case and embodiment, the specific embodiment of the present invention is elaborated.
Embodiment 1
The present invention, in concrete enforcement, is realized by following steps:
One, the processing of gac:
(1), bubble charcoal: method is, the deionized water of granularity 40-60 purpose specific conductivity≤40 μ s/cm for gac is soaked, standing 1.5-2.0h, abandon its upper strata floating matter, so repeatedly, (eliminating floating matter) no longer occur to the upper strata floating matter, then with centrifugal separator, gac is separated from solution, obtain brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio 1: 3(, be solid-to-liquid ratio 1: 3) join in enamel reactor, stir, become the gac mixing solutions, add again the nitric acid of mass concentration 65%-68% in the gac mixing solutions, the 1-2.0% that the nitric acid add-on is gac mixing solutions weight, slowly heat to 100 ℃-110 ℃, boil 4-5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is put into to centrifugal separator, start separating machine, gac is separated from mixing solutions, and the deionized water to adding specific conductivity≤40 μ s/cm in separator, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm, continue to separate 0.5-1.0h, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is the Sunmorl N 60S oxidation solution to be added in reactor to the gac that adds Sunmorl N 60S oxidation solution weight 1%-2% step 1 to process, open and stir, be heated to 70-80 ℃, insulation 0.5-3.0h, obtain mixing solutions;
(2), pressure filtration: adopt strainer to filter mixing solutions, the in-built filter stick 90-100 root that aperture 5-10 μ m is arranged of strainer, mixing solutions enters from strainer top under the pressure of 0.1-0.15Mpa, after the filter of filter stick essence, from the strainer bottom, flow out, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, and gac can reuse.
Embodiment 2
The present invention, in concrete enforcement, is realized by following steps:
One, the processing of gac:
(1), bubble charcoal: method is, the deionized water of granularity 40-60 purpose specific conductivity≤40 μ s/cm for gac is soaked, standing 100min, abandon its upper strata floating matter, so repeatedly, (eliminating floating matter) no longer occur to the upper strata floating matter, then with centrifugal separator, gac is separated from solution, obtain brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio 1: 3(, be solid-to-liquid ratio 1: 3) join in enamel reactor, stir, become the gac mixing solutions, add again the nitric acid of mass concentration 66% in the gac mixing solutions, the nitric acid add-on is 1.5% of gac mixing solutions weight, slowly heat to 105 ℃, boil 4.5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is put into to centrifugal separator, start separating machine, gac is separated from mixing solutions, and the deionized water to adding specific conductivity≤40 μ s/cm in separator, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm, continue to separate 50min, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is the Sunmorl N 60S oxidation solution to be added in reactor to the gac that adds Sunmorl N 60S oxidation solution weight 1.5% step 1 to process, open and stir, be heated to 75 ℃, insulation 2h, obtain mixing solutions;
(2), pressure filtration: adopt strainer to filter mixing solutions, the in-built filter stick 90-100 root that aperture 5-10 μ m is arranged of strainer, mixing solutions enters from strainer top under the pressure of 0.12Mpa, after the filter of filter stick essence, from the strainer bottom, flow out, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, and gac can reuse.
The present invention, through repetition test and actual the use, has obtained extraordinary technique effect, and gac can reuse 50-60 batch, greatly save raw material, reduced production cost, and after tested, the loss amount of palladium, bismuth reduces greatly, and relevant test case is as following table:
As can be seen from the table, the sodium gluconate solution of processing through this method, the content of Pd drops to 3ppm from 10ppm, descends nearly 70%; The content of Bi drops to 2ppm from 13ppm, descend nearly 76.9%, and solution is from the faint yellow water white transparency that becomes.
The present invention compared with prior art, has following outstanding useful technique effect:
1, the sodium gluconate solution that the catalytic oxidation of processing through the present invention is produced, heavy metal content sharply descends, and reaches the heavy metal content≤10ppm of product index requirement.
2, the sodium gluconate solution clear that the catalytic oxidation of processing through the present invention is produced, outer light quality is good.
What 3, the present invention adopted is the cocoanut active charcoal with high absorption capacity, and has passed through the gac pre-treatment, and use properties is good aborning, and can reuse 50-60 time, has improved the service efficiency of gac.
4, after the present invention processes, discarded charcoal absorption the most of heavy metal contained in former sodium gluconate solution, the content of heavy metal Pd in gac and Bi is respectively 0.01%, 0.03% after testing, and the Pd wherein contained has recovery value very much, and huge economic and social benefit is arranged.
Claims (3)
1. the method for a sodium gluconate solution of producing with the activated carbon treatment catalytic oxidation, is characterized in that, comprises the following steps:
One, the processing of gac:
(1), bubble charcoal: method is, gac is soaked with deionized water, and standing 1.5-2.0h, abandon its upper strata floating matter, so repeatedly, no longer occurs to the upper strata floating matter, then gac separated from solution, obtains brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio, to join in enamel reactor at 1: 3, stir, become the gac mixing solutions, then add the nitric acid of mass concentration 65%-68% in the gac mixing solutions, the 1-2.0% that the nitric acid add-on is gac mixing solutions weight, slowly heat to 100 ℃-110 ℃, boil 4-5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is separated, gac is separated from mixing solutions, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm with deionized water, continue to separate 0.5-1.0h, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is that the gac that adds Sunmorl N 60S oxidation solution weight 1%-2% step 1 to process the Sunmorl N 60S oxidation solution, open and stir, and is heated to 70-80 ℃, is incubated 0.5-3.0h, obtains mixing solutions;
(2), pressure filtration: mixing solutions is filtered under the pressure of 0.1-0.15Mpa, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, the gac recycling.
2. the method for the sodium gluconate solution of producing with the activated carbon treatment catalytic oxidation according to claim 1, is characterized in that, by following steps, realized:
One, the processing of gac:
(1), bubble charcoal: method is, the deionized water of granularity 40-60 purpose specific conductivity≤40 μ s/cm for gac is soaked, standing 1.5-2.0h, abandon its upper strata floating matter, so repeatedly, no longer occur to the upper strata floating matter, then with centrifugal separator, gac is separated from solution, obtain brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio, to join in enamel reactor at 1: 3, stir, become the gac mixing solutions, then add the nitric acid of mass concentration 65%-68% in the gac mixing solutions, the 1-2.0% that the nitric acid add-on is gac mixing solutions weight, slowly heat to 100 ℃-110 ℃, boil 4-5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is put into to centrifugal separator, start separating machine, gac is separated from mixing solutions, and the deionized water to adding specific conductivity≤40 μ s/cm in separator, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm, continue to separate 0.5-1.0h, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is the Sunmorl N 60S oxidation solution to be added in reactor to the gac that adds Sunmorl N 60S oxidation solution weight 1%-2% step 1 to process, open and stir, be heated to 70-80 ℃, insulation 0.5-3.0h, obtain mixing solutions;
(2), pressure filtration: adopt strainer to filter mixing solutions, the in-built filter stick 90-100 root that aperture 5-10 μ m is arranged of strainer, mixing solutions enters from strainer top under the pressure of 0.1-0.15Mpa, after the filter of filter stick essence, from the strainer bottom, flow out, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, the gac recycling.
3. the method for the sodium gluconate solution of producing with the activated carbon treatment catalytic oxidation according to claim 1, is characterized in that, by following steps, realized:
One, the processing of gac:
(1), bubble charcoal: method is, the deionized water of granularity 40-60 purpose specific conductivity≤40 μ s/cm for gac is soaked, standing 100min, abandon its upper strata floating matter, so repeatedly, no longer occur to the upper strata floating matter, then with centrifugal separator, gac is separated from solution, obtain brewed gac;
(2), boil charcoal: method is, by brewed gac, by gac and water weight ratio, to join in enamel reactor at 1: 3, stir, become the gac mixing solutions, then add the nitric acid of mass concentration 66% in the gac mixing solutions, the nitric acid add-on is 1.5% of gac mixing solutions weight, slowly heat to 105 ℃, boil 4.5h, stop heating, be cooled to 70 ℃ with tap water, stop stirring, more naturally be cooled to below 40 ℃, the cooked gac mixing solutions that obtains;
(3), wash charcoal: method is, well-done gac mixing solutions is put into to centrifugal separator, start separating machine, gac is separated from mixing solutions, and the deionized water to adding specific conductivity≤40 μ s/cm in separator, slowly rinse isolated gac to the specific conductivity of discharging washing lotion≤50 μ s/cm, continue to separate 50min, discharging, sampling analysis moisture, must wash the gac that charcoal is processed;
Two, sodium gluconate solution is processed, and method is:
(1), the heat treatment of Sunmorl N 60S oxidation solution: method is the Sunmorl N 60S oxidation solution to be added in reactor to the gac that adds Sunmorl N 60S oxidation solution weight 1.5% step 1 to process, open and stir, be heated to 75 ℃, insulation 2h, obtain mixing solutions;
(2), pressure filtration: adopt strainer to filter mixing solutions, the in-built filter stick 90-100 root that aperture 5-10 μ m is arranged of strainer, mixing solutions enters from strainer top under the pressure of 0.12Mpa, after the filter of filter stick essence, from the strainer bottom, flow out, obtain sodium gluconate solution and the gac of clear, sodium gluconate solution flows into the solvent or diluent pond, the gac recycling.
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| CN2013104200036A CN103467275A (en) | 2013-09-14 | 2013-09-14 | Catalytic oxidation production method of sodium gluconate liquid by means of activated carbon treatment |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1153166A (en) * | 1996-07-09 | 1997-07-02 | 桐乡市天融食品添加剂有限责任公司 | Method for preparing gluconate in presence of Bi-Pd/C metal catalyst |
| CN102337407A (en) * | 2011-08-06 | 2012-02-01 | 河南兴发精细化工有限公司 | Method for adsorbing palladium falling off in glucose oxidation process by active carbon |
| CN102698746A (en) * | 2012-06-18 | 2012-10-03 | 河南兴发精细化工有限公司 | Method for recovering lost noble metal catalyst at sodium gluconate oxidation section |
-
2013
- 2013-09-14 CN CN2013104200036A patent/CN103467275A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1153166A (en) * | 1996-07-09 | 1997-07-02 | 桐乡市天融食品添加剂有限责任公司 | Method for preparing gluconate in presence of Bi-Pd/C metal catalyst |
| CN102337407A (en) * | 2011-08-06 | 2012-02-01 | 河南兴发精细化工有限公司 | Method for adsorbing palladium falling off in glucose oxidation process by active carbon |
| CN102698746A (en) * | 2012-06-18 | 2012-10-03 | 河南兴发精细化工有限公司 | Method for recovering lost noble metal catalyst at sodium gluconate oxidation section |
Non-Patent Citations (1)
| Title |
|---|
| 黄伟等: "硝酸改性处理对活性炭性能的影响", 《生物质化学工程》 * |
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Application publication date: 20131225 |