CN103525462B - Lignite wax oxidizing and refining method - Google Patents
Lignite wax oxidizing and refining method Download PDFInfo
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- CN103525462B CN103525462B CN201310493914.1A CN201310493914A CN103525462B CN 103525462 B CN103525462 B CN 103525462B CN 201310493914 A CN201310493914 A CN 201310493914A CN 103525462 B CN103525462 B CN 103525462B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000007670 refining Methods 0.000 title claims abstract description 10
- 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 49
- 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 49
- 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 49
- 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 49
- 238000003756 stirring Methods 0.000 claims description 24
- 238000009897 hydrogen peroxide bleaching Methods 0.000 claims description 22
- 239000003381 stabilizer Substances 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 17
- 239000012752 auxiliary agent Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000000746 purification Methods 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
- 239000000203 mixture Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000012943 hotmelt Substances 0.000 claims description 8
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 238000005571 anion exchange chromatography Methods 0.000 claims description 5
- 239000000446 fuel Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000010898 silica gel chromatography Methods 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 1
- 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
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- 230000003647 oxidation Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 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
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- 230000007613 environmental effect Effects 0.000 description 4
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- 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
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- 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
- 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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- 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
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- 235000012254 magnesium hydroxide Nutrition 0.000 description 1
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- 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 from brown coal, extracts with organic solvent the waxy product obtained under certain condition, because its irreplaceable good characteristic is widely used in the fields such as daily use chemicals, casting, automobile.But make it be chocolate due to the material such as tricyclic diterpene, pentacyclic triterpene hydro carbons of aromizing in brown coal waxy stone, even if the montanin wax color after degreasing is still comparatively dark, this have impact on its range of application greatly.Therefore how to remove the oxide purification of dark material in montanin wax and become the research emphasis in montanin wax field, at present comparatively ripe and effective decoloring method is 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 process, but the incompleteness in view of technology makes its transformation efficiency can not reach absolutely (general peak rate of conversion is about 80 percent), 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 public sale related products at present, therefore also limit wideling popularize of this method, in addition the sulfuric acid lotion after using and water lotion will through complicated dialysis recyclings, and this has increased the weight of cost again indirectly, it is crucial that chromium drift products obtained therefrom more or less has the remnants of chromium element, which has limited its application in the high-end field such as daily use chemicals, food.Actively advocate today of construction " amphitypy society " in country, the cry of montanin wax Chrome-free oxide purification grows to even greater heights.Therefore, study hotspot and the development trend that new environmental protection oxidation system becomes this field is sought.
At present about the domestic article of montanin wax Chrome-free oxide purification and patent only a case each, Lee is precious just to be waited (" Li Baocai etc. the nitric acid oxidation of montanin wax refines [J]. 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 industrialization could not be realized.Although application number 201010535750.0 also discloses a kind of oxidative decoloration process for purification of montanin wax of Chrome-free, but it still also exists very large limitation: it adopts hydrogen peroxide and ammonia water mixture to be main drift agent, but repeatedly find after repeatability checking 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 operation controls difficulty, and it is excessive to add ammoniacal liquor pungent odour, and final effect exists misleading, because the wax after saponification is milky really, but more than higher than montanin wax fusing point (about about 80 DEG C) temperature, its final color is still darker, which illustrate chromophoric group or structure that the method can not destroy montanin wax inside effectively.And hydrogen peroxide very easily to decompose under the high temperature conditions when not adding stablizer be basic general knowledge, it slowly adds drift agent and stirs 1-4 hour under adopting 90-120 DEG C of condition, if shift decomposed drift agent not in time, the relative concentration adding drift agent after certainly will causing 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 the effective ways of non-chromium system oxide purification montanin wax are not still found.
Generally believe that a kind of SYNTHETIC OPTICAL WHITNER can only optionally some chromophoric group of attack, certain limit is existed to the raising of whiteness, and SYNTHETIC OPTICAL WHITNER also may generate new chromophoric group while the original chromophoric group of destruction.If several SYNTHETIC OPTICAL WHITNER destroying chromophoric group function different are combinationally used, so just can occur: can not only destroy original chromophoric group but also newborn chromophoric group can be made to become achromatic structure, such whiteness certainly will improve greatly.Apply in montanin wax oxide purification about the common bleaching of Peracetic Acid and hydrogen peroxide at present and have 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 excellent.
Three-stage process purification step of the present invention is as follows:
(1) according to degreasing montanin wax: Peracetic Acid: the mass ratio of Peracetic Acid auxiliary agent is the ratio preparation raw material of 1:0.2-0.3:0.005-0.02, first Peracetic Acid and Peracetic Acid auxiliary agent fully being mixed rear adjustment pH is 4-6, then mixed solution is divided into 3-5 part at 90-100 DEG C, adds stirring reaction 1-2 hour in degreasing montanin wax, front portion bleach residue is first isolated therebetween before newly adding Peracetic Acid and Peracetic Acid auxiliary agent mixed solution, finally obtained just drift section wax, for subsequent use;
(2) according to degreasing montanin wax: hydrogen peroxide: the mass ratio of hydrogen peroxide auxiliary agent is the ratio preparation raw material of 1:0.2-0.3:0.005-0.02, first hydrogen peroxide and hydrogen peroxide auxiliary agent fully being mixed rear adjustment pH is 8-10, then mixed solution is divided into 3-5 part stirring reaction 1-2 hour at 90-100 DEG C, front portion bleach residue is first isolated therebetween before newly adding hydrogen peroxide and hydrogen peroxide auxiliary agent mixed solution, finally the obtained section of drift again wax, washes for subsequent use;
(3) first dried at 60-70 DEG C by the multiple drift section wax after washing, stir therebetween in good time, when in multiple drift section wax during moisture content≤5%, raised temperature is to 90-100 DEG C, until after the whole hot melt of wax, normal temperature cools, and obtains refining montanin wax product.
The mass percent concentration of the Peracetic Acid used 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 used in the present invention is 25-30%, hydrogen peroxide auxiliary agent be 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 making 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 used for being separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, be that the ratio of 1:0.3-0.5 is mixed with gained free acid (butt) and magnesium hydroxide (analytical pure) according to mass ratio to be incorporated in 85 DEG C and to stir 5 minutes, cool levigate being and make BC-YC01 hydrogen peroxide bleaching stabilizer by oneself.
In the present invention, degreasing montanin wax is commercial degreasing montanin wax or degreasing montanin wax obtained according to a conventional method, product as obtained in reference patent application 201310047688.4 " in montanin wax, resin object deviates 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, with Peracetic Acid and hydrogen peroxide for main drift agent carrys out oxide purification montanin wax, very environmental protection; 2. the reaction times of the present invention is short, and bleaching whiteness is good, productive rate is also high; 3. to float products obtained therefrom close for the every quality index of products obtained therefrom of the present invention and traditional chromium, has to replace chromium and float on 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 the high-end field such as daily use chemicals, food; 5. the self-control hydrogen peroxide bleaching stabilizer used in the present invention is more a little than commercially available hydrogen peroxide bleaching stabilizer better effects if, and environmental sound of easily degrading; 6. the inventive method is simple, easy to operate, and technical feasibility, cost reduce, and obtained wax is excellent, 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 scope 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 drift control group is with reference to the light wax obtained by patent application 200810233581.8 " oxidization fine purification albefaction method of montanin wax " and measures its parameter.
embodiment 1
1, first 1kg degreasing montanin wax is added reactor, then 200g mass percent concentration be 15% peracetic acid soln and 5g water glass mixed dissolution after with NaOH adjust ph=4, reactor was added every 0.5 hour at 90 DEG C, each add-on is 1/3rd of total amount, stirring reaction 1.5 hours, front portion bleach residue is first isolated therebetween, finally obtained just drift section wax before newly adding mixed solution;
2, the first section of drift wax is inserted reactor, again 200g mass percent concentration be 25% superoxol and 5g ZJ-CH01 hydrogen peroxide bleaching stabilizer mixed dissolution after with NaOH adjust ph=8, reactor was added every 0.5 hour at 90 DEG C, each add-on is 1/3rd of total amount, stirring reaction 1.5 hours, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally the obtained section of drift again wax, washes for subsequent use;
3, washing is floated again to be laid in watch-glass and to insert in air dry oven after section wax slightly dries and dry, initial temperature is set to 60 DEG C, and stir in good time, when in drift wax, moisture content is 5%, raise the temperature inside the box to 90 DEG C, until after the whole hot melt 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 reactor, again 6kg mass percent concentration be 20% peracetic acid soln and 400g water-soluble chitosan mixed dissolution after with NaOH adjust ph=6, reactor was added every 0.4 hour at 95 DEG C, each add-on is 1/5th of total amount, stirring reaction 2 hours, front portion bleach residue is first isolated therebetween, finally obtained just drift section wax before newly adding mixed solution;
2, the first section of drift wax is inserted reactor, again 6kg mass percent concentration be 30% superoxol and 400g make by oneself after BC-YC01 hydrogen peroxide bleaching stabilizer mixed dissolution with NaOH adjust ph=10, and added reactor every 0.4 hour, each add-on is 1/5th of total amount, stirring reaction 2 hours at 95 DEG C, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally the obtained section of drift again wax, washes for subsequent use;
The preparation method wherein making 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 used for being separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, be that the ratio of 1:0.3 is mixed with gained free acid (butt) and magnesium hydroxide (analytical pure) according to mass ratio to be incorporated in 85 DEG C and to stir 5 minutes, cool levigate being and make BC-YC01 hydrogen peroxide bleaching stabilizer by oneself;
3, washing is floated again to be laid in watch-glass and to insert in air dry oven after section wax slightly dries and dry, initial temperature is set to 70 DEG C, and stir in good time, when floating moisture content=3% in wax, raise the temperature inside the box to 100 DEG C, until after the whole hot melt 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 reactor, again 2.5kg mass percent concentration be 18% peracetic acid soln and 100g disodium ethylene diamine tetraacetate mixed dissolution after with NaOH adjust ph=5, reactor was added every 0.4 hour at 100 DEG C, each add-on is 1/4th of total amount, stirring reaction 1 hour, front portion bleach residue is first isolated therebetween, finally obtained just drift section wax before newly adding mixed solution;
2, the first section of drift wax is inserted reactor, again 2.5kg mass percent concentration be 28% superoxol and 100g make by oneself after BC-YC01 hydrogen peroxide bleaching stabilizer mixed dissolution with NaOH adjust ph=9, and added reactor every 0.4 hour, each add-on is 1/4th of total amount, stirring reaction 1 hour at 100 DEG C, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally the obtained section of drift again wax, washes for subsequent use;
The preparation method wherein making 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 used for being separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, be that the ratio of 1:0.5 is mixed with gained free acid (butt) and magnesium hydroxide (analytical pure) according to mass ratio to be incorporated in 85 DEG C and to stir 5 minutes, cool levigate being and make BC-YC01 hydrogen peroxide bleaching stabilizer by oneself;
3, washing is floated again to be laid in watch-glass and to insert in air dry oven after section wax slightly dries and dry, initial temperature is set to 65 DEG C, and stir in good time, when in drift wax, moisture content is 4%, raise the temperature inside the box to 95 DEG C, until after the whole hot melt 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 reactor, again 6kg mass percent concentration be 20% peracetic acid soln and 200g water-soluble chitosan, after 200g disodium ethylene diamine tetraacetate mixed dissolution with NaOH adjust ph=6, reactor was added every 0.4 hour at 95 DEG C, each add-on is 1/5th of total amount, stirring reaction 2 hours, front portion bleach residue is first isolated therebetween, finally obtained just drift section wax before newly adding mixed solution;
2, the first section of drift wax is inserted reactor, again 6kg mass percent concentration be 30% superoxol and 200g make by oneself after BC-YC01 hydrogen peroxide bleaching stabilizer, 200gZJ-CH01 hydrogen peroxide bleaching stabilizer mixed dissolution with NaOH adjust ph=9, and added reactor every 0.4 hour, each add-on is 1/5th of total amount, stirring reaction 2 hours at 95 DEG C, before newly adding mixed solution, first isolate front portion bleach residue therebetween, finally the obtained section of drift again wax, washes for subsequent use;
The preparation method wherein making 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 used for being separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, be that the ratio of 1:0.4 is mixed with gained free acid (butt) and magnesium hydroxide (analytical pure) according to mass ratio to be incorporated in 85 DEG C and to stir 5 minutes, cool levigate being and make BC-YC01 hydrogen peroxide bleaching stabilizer by oneself;
3, washing is floated again to be laid in watch-glass and to insert in air dry oven after section wax slightly dries and dry, initial temperature is set to 70 DEG C, and stir in good time, when floating moisture content=3% in wax, raise the temperature inside the box to 100 DEG C, until after the whole hot melt of wax powder, move to normal temperature cooling, obtain refining montanin wax product, the present embodiment product property is as follows:
Claims (1)
1. an oxide purification method for montanin wax, is characterized in that: comprise the Peracetic Acid just section of drift, the hydrogen peroxide section of drift, oven dry hot melt section again, concrete purification step is as follows:
(1) the Peracetic Acid just section of drift: according to degreasing montanin wax: Peracetic Acid: the mass ratio of Peracetic Acid auxiliary agent is the ratio preparation raw material of 1:0.2-0.3:0.005-0.02, first Peracetic Acid and Peracetic Acid auxiliary agent fully being mixed rear adjustment pH is 4-6, then mixed solution is divided into 3-5 part at 90-100 DEG C, adds stirring reaction 1-2 hour in degreasing montanin wax, front portion bleach residue is first isolated therebetween before newly adding Peracetic Acid and Peracetic Acid auxiliary agent mixed solution, finally obtained just drift section wax, for subsequent use;
(2) the hydrogen peroxide section of drift again: according to degreasing montanin wax: hydrogen peroxide: the mass ratio of hydrogen peroxide auxiliary agent is the ratio preparation raw material of 1:0.2-0.3:0.005-0.02, first hydrogen peroxide and hydrogen peroxide auxiliary agent fully being mixed rear adjustment pH is 8-10, then mixed solution is divided into 3-5 part at 90-100 DEG C, adds stirring reaction 1-2 hour in first drift section wax, front portion bleach residue is first isolated therebetween before newly adding hydrogen peroxide and hydrogen peroxide auxiliary agent mixed solution, finally the obtained section of drift again wax, washes for subsequent use;
(3) dry hot melt section: first dried at 60-70 DEG C by the multiple drift section wax after washing, stir therebetween, when in multiple drift section wax during moisture content≤5%, raised temperature is to 90-100 DEG C, until after the whole hot melt of wax, normal temperature cools, and obtains refining montanin wax product;
The mass percent concentration of described Peracetic Acid is 15-20%;
Described Peracetic Acid auxiliary agent is one or several the mixture in water-soluble chitosan, water glass, ethylenediamine tetraacetic acid (EDTA);
The mass percent concentration of described hydrogen peroxide is 25-30%;
Described hydrogen peroxide auxiliary agent is BC-YC01 hydrogen peroxide bleaching stabilizer and/or ZJ-CH01 hydrogen peroxide bleaching stabilizer;
The preparation method of described BC-YC01 hydrogen peroxide bleaching stabilizer is: with reference to periodical literature: " Li Baocai etc. anion-exchange chromatography and silica gel column chromatography are used for being separated [J] of montanin wax group composition. chemistry of fuel journal; 1988; 16(1): 31. " separation method of Free Acid obtains free acid, be that the ratio of 1 ︰ 0.3-0.5 is mixed with gained free acid butt and analytical pure magnesium hydroxide according to mass ratio to be incorporated in 85 DEG C and to stir 5 minutes, cool and levigately namely obtain BC-YC01 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 CN103525462A (en) | 2014-01-22 |
| CN103525462B true CN103525462B (en) | 2015-05-20 |
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| CN201310493914.1A Active CN103525462B (en) | 2013-10-21 | 2013-10-21 | Lignite wax oxidizing and refining method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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