CN103525462A - Lignite wax oxidizing and refining method - Google Patents
Lignite wax oxidizing and refining method Download PDFInfo
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- CN103525462A CN103525462A CN201310493914.1A CN201310493914A CN103525462A CN 103525462 A CN103525462 A CN 103525462A CN 201310493914 A CN201310493914 A CN 201310493914A CN 103525462 A CN103525462 A CN 103525462A
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- hydrogen peroxide
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007670 refining Methods 0.000 title claims abstract description 11
- 239000003077 lignite Substances 0.000 title abstract description 8
- 230000001590 oxidative effect Effects 0.000 title abstract description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 56
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 5
- MKYLOMHWHWEFCT-UHFFFAOYSA-N Manthidine Natural products C1C2=CC=3OCOC=3C=C2C2C3=CC(OC)C(O)CC3N1C2 MKYLOMHWHWEFCT-UHFFFAOYSA-N 0.000 claims description 52
- SNFRINMTRPQQLE-JQWAAABSSA-N Montanin Chemical compound O[C@H]([C@@]1(CO)O[C@H]1[C@H]1[C@H]2O3)[C@]4(O)C(=O)C(C)=C[C@H]4[C@]11OC3(CCCCCCCCCCC)O[C@@]2(C(C)=C)C[C@H]1C SNFRINMTRPQQLE-JQWAAABSSA-N 0.000 claims description 52
- SNFRINMTRPQQLE-OFGNMXNXSA-N Montanin Natural products O=C1[C@@]2(O)[C@@H](O)[C@@]3(CO)O[C@H]3[C@@H]3[C@H]4[C@@]5(C(=C)C)O[C@](CCCCCCCCCCC)(O4)O[C@@]3([C@H](C)C5)[C@@H]2C=C1C SNFRINMTRPQQLE-OFGNMXNXSA-N 0.000 claims description 52
- QTZPBQMTXNEKRX-UHFFFAOYSA-N Voacristine pseudoindoxyl Natural products N1C2=CC=C(OC)C=C2C(=O)C21CCN(C1)C3C(C(C)O)CC1CC32C(=O)OC QTZPBQMTXNEKRX-UHFFFAOYSA-N 0.000 claims description 52
- 238000007667 floating Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 23
- 238000009897 hydrogen peroxide bleaching Methods 0.000 claims description 20
- 238000000746 purification Methods 0.000 claims description 20
- 239000003381 stabilizer Substances 0.000 claims description 20
- 239000012752 auxiliary agent Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000005238 degreasing Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000007844 bleaching agent Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012943 hotmelt Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052804 chromium Inorganic materials 0.000 abstract description 8
- 239000011651 chromium Substances 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 239000002253 acid Substances 0.000 description 14
- 238000004090 dissolution Methods 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 5
- 239000000347 magnesium hydroxide Substances 0.000 description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 4
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 4
- 238000005571 anion exchange chromatography Methods 0.000 description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000010898 silica gel chromatography Methods 0.000 description 4
- 238000004061 bleaching Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
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- 229930004069 diterpene Natural products 0.000 description 1
- 150000004141 diterpene derivatives Chemical class 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000012254 magnesium hydroxide Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- -1 triterpene hydro carbons Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Detergent Compositions (AREA)
Abstract
The invention discloses a lignite wax oxidizing and refining method which comprises the following steps: on the basis of taking degreased lignite wax as a raw material, refining the lignite wax by using a sectional method, firstly, performing primary rinsing by using peracetic acid and assistant, subsequently performing secondary rinsing by using hydrogen peroxide and hydrogen peroxide assistant, and finally drying and preparing a refined lignite wax product in a hot melting mode. The method disclosed by the invention is simple, feasible in technique, environment-friendly and energy-saving, the prepared wax is excellent in quality, and the method is an effective method for oxidizing and refining lignite wax of a non-chromium system.
Description
Technical field
The present invention relates to a kind of oxide purification method, specifically a kind of environmental protection oxide purification method of montanin wax.
Background technology
Montanin wax is with the organic solvent wax product that extraction obtains from brown coal under certain condition, because its irreplaceable good characteristic is widely used in the fields such as daily use chemicals, casting, automobile.But because the materials such as the tricyclic diterpene of aromizing in brown coal waxy stone, pentacyclic triterpene hydro carbons make it be chocolate, even if the montanin wax color after degreasing is still darker, this has affected its range of application greatly.Therefore how removing the oxide purification of dark material in montanin wax becomes the research emphasis in montanin wax field, at present comparatively ripe and effectively decoloring method be still chromic anhydride, chromic acid and the method for oxidation of dichromic, but there is many defects and deficiency, first be that chrome liquor used is rich in heavy metal chromium element, chromium waste liquid industry after oxidation generally adopts electrolytic regeneration to process, but in view of the incompleteness of technology makes its transformation efficiency can not reach absolutely (general peak rate of conversion is 80 percent left and right), so in fact still will constantly add new chrome liquor in whole production chain, and electrolyzer cost is high and highly confidential, there is no at present public sale related products, therefore also limited wideling popularize of this method, in addition the sulfuric acid lotion after using and water lotion will be through complicated dialysis recyclings, and this has increased the weight of again cost indirectly, most critical be that chromium floats the remnants that products obtained therefrom more or less has chromium element, this has limited its application in high-end fields such as daily use chemicals, food.The today of actively advocating construction " amphitypy society " in country, the cry of montanin wax Chrome-free oxide purification grows to even greater heights.Therefore, seek study hotspot and the development trend that new environmental protection oxidation system becomes this field.
At present only a case each about domestic article and the patent of montanin wax Chrome-free oxide purification, Lee is precious just to be waited (" Li Baocai etc. the nitric acid oxidation refining [J] of montanin wax. Jiangxi humic acids; 1987; (1): 29-35. ") once attempted nitric acid oxidation and refine montanin wax, consequently product can not decolour completely, and easily cause environmental pollution, therefore could not realize industrialization.Although application number 201010535750.0 has also been announced a kind of oxidative decoloration process for purification of montanin wax of Chrome-free, but it still exists very large limitation: it adopts hydrogen peroxide and ammonia water mixture is the main agent of floating, but repeatedly after repeatability checking, find to there will be obvious saponification reaction in the method experimentation, montanin wax can become spumescence and expand, if solvent slightly adds and too fastly can cause vigorous splash, it is larger that difficulty is controlled in operation, and add ammoniacal liquor pungent odour excessive, and that final effect exists is misleading, because the wax after saponification is milky really, but higher than montanin wax fusing point (approximately 80 ℃ of left and right) more than temperature, its final color is still darker, this has illustrated that the method can not destroy chromophoric group or the structure of montanin wax inside effectively.And it has been basic general knowledge that hydrogen peroxide very easily decomposes when not adding stablizer under hot conditions, it adopts under 90-120 ℃ of condition and slowly adds and float agent stirring 1-4 hour, if shift not in time the decomposed agent of floating, after certainly will causing, add and float that the relative concentration of agent is more and more less and hydrogen peroxide retention time is too short, so have a strong impact on its oxidation effectiveness.The problem of core is the acid hard montanin wax of light color that this method can not obtain real meaning, is more not suitable with the deep processing of montanin wax.Therefore still do not find the effective ways of non-chromium system oxide purification montanin wax.
Generally believe optionally some chromophoric group of attack of a kind of SYNTHETIC OPTICAL WHITNER, the raising of whiteness is existed to certain limit, and SYNTHETIC OPTICAL WHITNER also may generate new chromophoric group when destroying original chromophoric group.If be used in combination destroying the different several SYNTHETIC OPTICAL WHITNER of chromophoric group function, so just can occur: not only can destroy original chromophoric group but also can make newborn chromophoric group become achromatic structure, whiteness certainly will improve greatly like this.Combination bleaching application in montanin wax oxide purification about Peracetic Acid and hydrogen peroxide at present has no report.
Summary of the invention
For the shortcomings and deficiencies of prior art, the invention provides a kind of method of simple to operate, technical feasibility, energy-conserving and environment-protective, montanin wax oxide purification that wax is good.
Three-stage process purification step of the present invention is as follows:
(1) according to degreasing montanin wax: Peracetic Acid: the ratio that the mass ratio of Peracetic Acid auxiliary agent is 1:0.2-0.3:0.005-0.02 is prepared raw material, first Peracetic Acid and Peracetic Acid auxiliary agent fully being mixed to rear adjusting pH is 4-6, then mixed solution is divided into 3-5 part and at 90-100 ℃, adds stirring reaction 1-2 hour in degreasing montanin wax, before newly adding Peracetic Acid and Peracetic Acid auxiliary agent mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax, standby;
(2) according to degreasing montanin wax: hydrogen peroxide: the ratio that the mass ratio of hydrogen peroxide auxiliary agent is 1:0.2-0.3:0.005-0.02 is prepared raw material, first hydrogen peroxide and hydrogen peroxide auxiliary agent fully being mixed to rear adjusting pH is 8-10, then mixed solution is divided into 3-5 part stirring reaction 1-2 hour at 90-100 ℃, before newly adding hydrogen peroxide and hydrogen peroxide auxiliary agent mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
(3) section of the floating wax of answering after washing is first dried at 60-70 ℃, stir therebetween in good time, in the section of floating wax again, during moisture content≤5%, rising temperature is to 90-100 ℃, until after the whole hot melts of wax, normal temperature is cooling, obtains refining montanin wax product.
The mass percent concentration of the Peracetic Acid of using in the present invention is 15-20%; Peracetic Acid auxiliary agent be in water-soluble chitosan, water glass, disodium ethylene diamine tetraacetate one or several arbitrarily than mixture.
The mass percent concentration of the hydrogen peroxide using in the present invention is 25-30%, and hydrogen peroxide auxiliary agent is a kind of in self-control BC-YC01 hydrogen peroxide bleaching stabilizer, commercially available ZJ-CH01 hydrogen peroxide bleaching stabilizer or two kinds arbitrarily than mixture.
The preparation method who makes BC-YC01 hydrogen peroxide bleaching stabilizer in the present invention by oneself is: with reference to periodical literature: " Li Baocai etc. anion-exchange chromatography and silica gel column chromatography are for separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, mixed 85 ℃ of stirrings 5 minutes that are incorporated in of the ratio that is 1:0.3-0.5 according to mass ratio with gained free acid (butt) and magnesium hydroxide (analytical pure), the cooling levigate self-control BC-YC01 hydrogen peroxide bleaching stabilizer that is.
In the present invention, degreasing montanin wax is commercial degreasing montanin wax or the degreasing montanin wax making according to a conventional method, as the product making with reference to patent application 201310047688.4 " in montanin wax resin object deviate from method "; Peracetic Acid, hydrogen peroxide, water-soluble chitosan, water glass, magnesium hydroxide, disodium ethylene diamine tetraacetate, ZJ-CH01 hydrogen peroxide bleaching stabilizer are commercial reagent.
Feature of the present invention is: 1. the present invention has stopped the use of pollutent chrome liquor, take Peracetic Acid and hydrogen peroxide to float agent and come oxide purification montanin wax, very environmental protection as main; 2. the reaction times of the present invention short, bleaching whiteness good, productive rate is also high; 3. the every quality index of products obtained therefrom of the present invention and traditional chromium float products obtained therefrom and approach, and have to replace chromium and float on the status feasibility in montanin wax bleaching; 4. products obtained therefrom heavy metal free chromium element of the present invention is remaining, has expanded its application in high-end fields such as daily use chemicals, food; 5. the self-control hydrogen peroxide bleaching stabilizer using in the present invention is more a little than commercially available hydrogen peroxide bleaching stabilizer better effects if, and the environmental sound of easily degrading; 6. the inventive method is simple, easy to operate, technical feasibility, cost, and the wax making is good, is a kind of effective ways of non-chromium system oxide purification montanin wax.
embodiment
?below by embodiment, the present invention is described in further detail, but protection domain of the present invention is not limited to described content.In all embodiment data, fusing point, acid number, soap value test method are with reference to GB/T 2559-2005 below, and chromium floats control group to be with reference to the prepared light wax of patent application 200810233581.8 " oxidization fine purification albefaction method of montanin wax " and to measure its parameter.
embodiment 1
1, first 1kg degreasing montanin wax is added to reactor, then after the peracetic acid soln that is 15% 200g mass percent concentration and 5g water glass mixed dissolution, with NaOH, regulate pH value=4, at 90 ℃, every 0.5 hour, add reactor, each add-on is total amount 1/3rd, stirring reaction 1.5 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax;
2, just the section of floating wax is inserted reactor, after the superoxol that is 25% 200g mass percent concentration again and 5g ZJ-CH01 hydrogen peroxide bleaching stabilizer mixed dissolution, with NaOH, regulate pH value=8, at 90 ℃, every 0.5 hour, add reactor, each add-on is total amount 1/3rd, stirring reaction 1.5 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
3, by washing again the section of floating wax after slightly drying, be laid in watch-glass and insert in air dry oven and dry, initial temperature is set to 60 ℃, and stir in good time, when in floating wax, moisture content is 5%, rising the temperature inside the box to 90 ℃, until after the whole hot melts of wax powder, move to normal temperature cooling, obtain refining montanin wax product, the present embodiment product property is as follows:
embodiment2
1, first 20kg degreasing montanin wax is added to reactor, after the peracetic acid soln that is 20% 6kg mass percent concentration again and 400g water-soluble chitosan mixed dissolution, with NaOH, regulate pH value=6, at 95 ℃, every 0.4 hour, add reactor, each add-on is total amount 1/5th, stirring reaction 2 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax;
2, just the section of floating wax is inserted reactor, after the superoxol that is 30% 6kg mass percent concentration again and 400g self-control BC-YC01 hydrogen peroxide bleaching stabilizer mixed dissolution, with NaOH, regulate pH value=10, and every 0.4 hour, add reactor, each add-on is total amount 1/5th, at 95 ℃, stirring reaction is 2 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
The preparation method who wherein makes BC-YC01 hydrogen peroxide bleaching stabilizer by oneself is: with reference to periodical literature: " Li Baocai etc. anion-exchange chromatography and silica gel column chromatography are for separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, mixed 85 ℃ of stirrings 5 minutes that are incorporated in of the ratio that is 1:0.3 according to mass ratio with gained free acid (butt) and magnesium hydroxide (analytical pure), the cooling levigate self-control BC-YC01 hydrogen peroxide bleaching stabilizer that is;
3, by washing again the section of floating wax after slightly drying, be laid in watch-glass and insert in air dry oven and dry, initial temperature is set to 70 ℃, and stir in good time, in floating wax during moisture content=3%, rising the temperature inside the box to 100 ℃, until after the whole hot melts of wax powder, move to normal temperature cooling, obtain refining montanin wax product, the present embodiment product property is as follows:
embodiment3
1, first 10kg degreasing montanin wax is added to reactor, after the peracetic acid soln that is 18% 2.5kg mass percent concentration again and 100g disodium ethylene diamine tetraacetate mixed dissolution, with NaOH, regulate pH value=5, at 100 ℃, every 0.4 hour, add reactor, each add-on is total amount 1/4th, stirring reaction 1 hour, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax;
2, just the section of floating wax is inserted reactor, after the superoxol that is 28% 2.5kg mass percent concentration again and 100g self-control BC-YC01 hydrogen peroxide bleaching stabilizer mixed dissolution, with NaOH, regulate pH value=9, and every 0.4 hour, add reactor, each add-on is total amount 1/4th, at 100 ℃, stirring reaction is 1 hour, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
The preparation method who wherein makes BC-YC01 hydrogen peroxide bleaching stabilizer by oneself is: with reference to periodical literature: " Li Baocai etc. anion-exchange chromatography and silica gel column chromatography are for separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, mixed 85 ℃ of stirrings 5 minutes that are incorporated in of the ratio that is 1:0.5 according to mass ratio with gained free acid (butt) and magnesium hydroxide (analytical pure), the cooling levigate self-control BC-YC01 hydrogen peroxide bleaching stabilizer that is;
3, by washing again the section of floating wax after slightly drying, be laid in watch-glass and insert in air dry oven and dry, initial temperature is set to 65 ℃, and stir in good time, when in floating wax, moisture content is 4%, rising the temperature inside the box to 95 ℃, until after the whole hot melts of wax powder, move to normal temperature cooling, obtain refining montanin wax product, the present embodiment product property is as follows:
embodiment4
1, first 20kg degreasing montanin wax is added to reactor, after the peracetic acid soln that is 20% 6kg mass percent concentration again and 200g water-soluble chitosan, 200g disodium ethylene diamine tetraacetate mixed dissolution, with NaOH, regulate pH value=6, at 95 ℃, every 0.4 hour, add reactor, each add-on is total amount 1/5th, stirring reaction 2 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax;
2, just the section of floating wax is inserted reactor, after the superoxol that is 30% 6kg mass percent concentration again and 200g self-control BC-YC01 hydrogen peroxide bleaching stabilizer, 200gZJ-CH01 hydrogen peroxide bleaching stabilizer mixed dissolution, with NaOH, regulate pH value=9, and every 0.4 hour, add reactor, each add-on is total amount 1/5th, at 95 ℃, stirring reaction is 2 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
The preparation method who wherein makes BC-YC01 hydrogen peroxide bleaching stabilizer by oneself is: with reference to periodical literature: " Li Baocai etc. anion-exchange chromatography and silica gel column chromatography are for separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, mixed 85 ℃ of stirrings 5 minutes that are incorporated in of the ratio that is 1:0.4 according to mass ratio with gained free acid (butt) and magnesium hydroxide (analytical pure), the cooling levigate self-control BC-YC01 hydrogen peroxide bleaching stabilizer that is;
3, by washing again the section of floating wax after slightly drying, be laid in watch-glass and insert in air dry oven and dry, initial temperature is set to 70 ℃, and stir in good time, in floating wax during moisture content=3%, rising the temperature inside the box to 100 ℃, until after the whole hot melts of wax powder, move to normal temperature cooling, obtain refining montanin wax product, the present embodiment product property is as follows:
Claims (5)
1. an oxide purification method for montanin wax, is characterized in that: comprise Peracetic Acid just the section of floating, hydrogen peroxide again the section of floating, dry hot melt section, concrete purification step is as follows:
(1) the first section of floating of Peracetic Acid: according to degreasing montanin wax: Peracetic Acid: the ratio that the mass ratio of Peracetic Acid auxiliary agent is 1:0.2-0.3:0.005-0.02 is prepared raw material, first Peracetic Acid and Peracetic Acid auxiliary agent fully being mixed to rear adjusting pH is 4-6, then mixed solution is divided into 3-5 part and at 90-100 ℃, adds stirring reaction 1-2 hour in degreasing montanin wax, before newly adding Peracetic Acid and Peracetic Acid auxiliary agent mixed solution, first isolate front portion bleach residue therebetween, finally make the just section of floating wax, standby;
(2) the hydrogen peroxide section of floating again: according to degreasing montanin wax: hydrogen peroxide: the ratio that the mass ratio of hydrogen peroxide auxiliary agent is 1:0.2-0.3:0.005-0.02 is prepared raw material, first hydrogen peroxide and hydrogen peroxide auxiliary agent fully being mixed to rear adjusting pH is 8-10, then mixed solution is divided into 3-5 part stirring reaction 1-2 hour at 90-100 ℃, before newly adding hydrogen peroxide and hydrogen peroxide auxiliary agent mixed solution, first isolate front portion bleach residue therebetween, finally make the section of floating wax again, wash standby;
(3) dry hot melt section: the section of the floating wax of answering after washing is first dried at 60-70 ℃, stir, during moisture content≤5%, rising temperature is to 90-100 ℃, until after the whole hot melts of wax, normal temperature is cooling, obtains refining montanin wax product in the section of floating wax again therebetween.
2. the oxide purification method of montanin wax according to claim 1, is characterized in that: the mass percent concentration of Peracetic Acid is 15-20%.
3. the oxide purification method of montanin wax according to claim 1, is characterized in that: Peracetic Acid auxiliary agent is one or several the mixture in water-soluble chitosan, water glass, ethylenediamine tetraacetic acid (EDTA).
4. the oxide purification method of montanin wax according to claim 1, is characterized in that: the mass percent concentration of hydrogen peroxide is 25-30%.
5. the oxide purification method of montanin wax according to claim 1, is characterized in that: hydrogen peroxide auxiliary agent is BC-YC01 hydrogen peroxide bleaching stabilizer and/or ZJ-CH01 hydrogen peroxide bleaching stabilizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310493914.1A CN103525462B (en) | 2013-10-21 | 2013-10-21 | Lignite wax oxidizing and refining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310493914.1A CN103525462B (en) | 2013-10-21 | 2013-10-21 | Lignite wax oxidizing and refining method |
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| Publication Number | Publication Date |
|---|---|
| CN103525462A true CN103525462A (en) | 2014-01-22 |
| CN103525462B CN103525462B (en) | 2015-05-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104820027A (en) * | 2015-04-14 | 2015-08-05 | 昆明理工大学 | Gas chromatographic fingerprint detection method of resin-removed montan wax |
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| SU757587A1 (en) * | 1978-10-24 | 1980-08-23 | Semnovskij Z Gornogo Voska | Method of refining tar-free lignite wax |
| CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
| CN101575820A (en) * | 2009-06-08 | 2009-11-11 | 昆明理工大学 | Method for removing metal ions of paper pulp and bleaching |
| CN102587186A (en) * | 2012-03-20 | 2012-07-18 | 昆明理工大学 | Method for bleaching dendrocalamus giganteus chemical pulp |
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| SU757587A1 (en) * | 1978-10-24 | 1980-08-23 | Semnovskij Z Gornogo Voska | Method of refining tar-free lignite wax |
| CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
| CN101575820A (en) * | 2009-06-08 | 2009-11-11 | 昆明理工大学 | Method for removing metal ions of paper pulp and bleaching |
| CN102587186A (en) * | 2012-03-20 | 2012-07-18 | 昆明理工大学 | Method for bleaching dendrocalamus giganteus chemical pulp |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104820027A (en) * | 2015-04-14 | 2015-08-05 | 昆明理工大学 | Gas chromatographic fingerprint detection method of resin-removed montan wax |
| CN104820027B (en) * | 2015-04-14 | 2016-11-16 | 昆明理工大学 | A kind of Gas Chromatography Fingerprint detection method of deresination lignite wax |
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| CN103525462B (en) | 2015-05-20 |
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