CN107903946B - A kind of preparation method of montanin wax resin distillate - Google Patents
A kind of preparation method of montanin wax resin distillate Download PDFInfo
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- CN107903946B CN107903946B CN201710998055.XA CN201710998055A CN107903946B CN 107903946 B CN107903946 B CN 107903946B CN 201710998055 A CN201710998055 A CN 201710998055A CN 107903946 B CN107903946 B CN 107903946B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/38—Chemical modification of petroleum
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/40—Physical treatment of waxes or modified waxes, e.g. granulation, dispersion, emulsion, irradiation
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Abstract
The invention discloses a kind of preparation methods of montanin wax resin distillate, belong to agriculture chemistry technical field.It is specifically a kind of by montanin wax resin through oxidation, degradation, evaporation, concentration, condensation and etc. be made distillate process and a kind of new way for efficiently being utilized montanin wax resin " turning waste into wealth ".Preparation-obtained distillation liquid product seedling good child-rearing, in terms of can obtain good produce effects, show the extremely low active high characteristic of active principle content, with significant advantage in terms of the exploitation of montanin wax resin high-end product, promoting product, show huge market prospects, and Nonpoisonous, non-environmental-pollution, flexible and convenient to use.In addition, its process flow is simple, energy conservation and environmental protection, high production efficiency, safe operability are strong, advantage of lower cost, it is easy to spread.
Description
Technical field
The present invention relates to a kind of preparation methods of montanin wax resin distillate, belong to agriculture chemistry technical field.
Background technique
Montanin wax (Montan Wax) is a kind of rare mine extracted from the young coal such as lignite, peat with organic solvent
It produces, is called lignite wax or peat wax again because source is different.Montanin wax resin refers to the general name of the resin component in montanin wax.?
In montanin wax technical field, montanin wax crude product is generally divided into three basic components: pure wax (accounting for about 60-70%), resin are (about
Account for 20-30%) and asphalt (accounting for about 5-10%);Pure wax belongs to " effective component " in montanin wax processing and utilization, and resin and ground
Pitch is considered as interfering " harmful components " of its performance, and the content of especially resin is larger so that its influence is especially prominent;Therefore,
In order to give full play to the excellent performance of montanin wax, it usually needs as far as possible by resin therein and bitumen component and pure wax component
Ground separation, by resin component from removing in montanin wax crude product be always one of committed step in montanin wax process for refining.But by
The developmental research to montanin wax resin is ignored in people for a long time, its many potential value is caused not excavated deeply,
Therefore it is mostly handled at present as " waste ", the by-product of " pile up like a mountain " also becomes puzzlement montanin wax in continuous production
The a great problem of enterprise.Since montanin wax resin component is extremely complex and the separating difficulty of monomer compound is big, lead
Cause its advances of Basic Research very slow, so research for application and development is also difficult to meet the real needs of enterprise.
Seminar belonging to inventor is dedicated to the basic and applied research of montanin wax resin for a long time, also obtains one at present
A little more valuable research achievements, such as: montanin wax resin is difficult to activity therein under the premise of without any processing
Ingredient is used, this is also the basic reason that montanin wax resin cannot efficiently use for a long time;If but being carried out to it appropriate
Activation, degradation, modified, active constituent can be able to " discharge ", so that it may obtain good application in numerous areas
Effect.Applied patent " a kind of Preparation method and use of lignite wax resin modified object " (application number before
201610651169.2) provide a kind of method of montanin wax resin oxidative degradation, modification, particularly as be resin is added to by
Oxidative degradation is carried out in the reaction solution of a variety of oxidant compositions, later solid-liquor separation, obtains liquid object (oxidation waste liquid) and solid-state
The resin modified object that can be used for ink adhesive is finally made in object, solid with the reaction of other compounds again.The patented technology is given
Principal degradation modified product (solid) after montanin wax resin oxidative degradation provides an advantageous industrialized utilization
Mode and field.Another patent " a kind of resin activated modification liquid of lignite wax and its production method and purposes " (application number
Secondary catabolite after 201610647937.7) then providing montanin wax resin oxidative degradation --- oxidation waste liquid (or change
Property liquid) application method in fields such as veterinary drug, agriculturals.It is above also only opening for the potential added value development and utilization of montanin wax resin
End or even " tip of the iceberg ".
Although the method for disclosing montanin wax resin oxidative degradation in above-mentioned two patent texts, in view of working as
When research level and experience level, still there is significant limitation.Although dividing for example, using secondary solvent resin
Scattered property makees improvement processing, but auxiliary agent type and proportion are not screened and optimized to the greatest extent, therefore its effecting reaction is sent out
Raw degree and its range are not optimal;At that time in view of the problems such as oxidant is left and desalination technology is unqualified, selecting
Directly eliminate that oxidation activity is higher, effect better inorganic oxidizer when selecting oxidant, and oxidant is left and desalination now
The problem of be resolved, make inorganic oxidizer become a kind of selection;Two above factor strong influence catabolite
The type and quantity of yield and active constituent.Therefore, in view of currently comprehensive development and utilization to montanin wax resin it is horizontal it is relatively low with
Its potential higher contradiction status of Development volue, the production technology upgrading or even high added value utilize to montanin wax resin are new
The exploitation and its application of product just seem especially urgent.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of montanin wax resin distillate, and montanin wax resin is carried out
Effective oxidative degradation, while water-soluble product (modification liquid) and insoluble modification solid have been obtained, modification liquid is carried out
Being concentrated by evaporation obtained evaporation condensate is montanin wax resin distillate, this method be also enhancing montanin wax resin water solubility with
And excavate a kind of effective way of its potential added value.
Montanin wax resin distillate of the present invention the preparation method is as follows:
(1) montanin wax resin is placed in reaction kettle, by reaction promoter: montanin wax resin=1:3-5 mass ratio is added anti-
Auxiliary agent is answered, is stirred and evenly mixed under conditions of 70-90 DEG C.
(2) after the completion of step (1), by montanin wax resin: reaction solution=1:8-16 mass ratio is added instead into reaction kettle
Liquid is answered, is then stirred to react 2-3h under conditions of 80-100 DEG C, to be cooled to room temperature after reaction, 1-2h is stood and carries out liquid
Gu separation.
(3) taking-up is quiet is centrifuged, and obtains supernatant, supernatant is carried out vacuum filter, filtered fluid changes for resin
Property liquid stoste;By modification liquid stoste, vacuum evaporation is evaporated to the one third of original volume under conditions of 50-70 DEG C
Gas condensation after obtained condensate liquid be montanin wax resin distillate.
The reaction promoter the preparation method comprises the following steps: press Tween 80: ethyl alcohol: propandiol butyl ether=1:1-2:3-5 mass ratio will
Three mixes in advance, obtains mixture, is then configured to the aqueous solution that mass fraction is 25-40%.
Reaction solution described in step (2) the preparation method comprises the following steps: press sodium peroxydisulfate: sodium dichromate: acid solution=1:1-2:
Two kinds of salt are completely dissolved in the acid solution of heat by the mass ratio of 10-15, and wherein acid solution is containing 10% mass point
The aqueous solution of the ferrous sulfate of several sulfuric acid and 4% mass fraction.
Preferably, the speed of agitator stirred in step (1) of the present invention is 50-60r/min, mixing time 20-30min.
Preferably, speed of agitator is 80-100r/min in step (2) of the present invention.
Preferably, the condition being centrifugated in step (3) of the present invention are as follows: 4000-5000r/min is centrifugated 6-10min.
Beneficial effects of the present invention are as follows:
(1) production method of montanin wax resin distillate provided by the present invention be combine closely montanin wax resin itself
Feature and application direction, the completely new process route of one kind obtained on the basis of breaking through original technology defect and bottleneck, work
Skill process is simple, energy conservation and environmental protection, high production efficiency, safe operability are strong, advantage of lower cost, has good promotion price
Value.Firstly, selective oxidation activity of the present invention is higher, the better inorganic oxidizer of effect forms the oxidation system of the technique;Oxidation
Agent is influence factor most crucial in distillate production technology, the prior art (201610651169.2 He of number of patent application
201610647937.7) oxidant used itself or its catabolite may be volatilized to enter into distillate with steam, right
Product pollutes;Present invention process uses inorganic oxidizer completely, itself or catabolite will not be volatized into steam
Into distillate, the pure of product ensure that;The raising of oxidation system oxidation susceptibility is conducive to product active ingredient content and kind
The increase of class, helps to improve product quality and benefit;The gas generated in present invention process Oxidative Degradation Process is less and slow
Slowly, it avoids bulk gas in the prior art and generates bring security risk rapidly.Secondly, type to resin secondary solvent and
Proportion has re-started screening and optimization, and the dispersibility of resin is further improved in reaction system, and effecting reaction occurs
Degree and range are greatly improved, and are conducive to increase the yield of catabolite and the type and quantity of active constituent.
(2) the montanin wax resin distillation liquid product that the present invention is prepared is equal in seedling good child-rearing and two aspect of increasing crop yield
Obtain it is good produce effects, and it is Nonpoisonous, non-environmental-pollution, flexible and convenient to use, inject new vitality to develop green agriculture, be also agriculture
People's increasing both production and income provides a kind of new agricultural supplie selection.Although being made with the prior art (number of patent application 201610647937.7)
Standby resin modified liquid purposes is similar, and there is certain relevance in substance source, but there are essential distinctions for two kinds of products: firstly, steaming
Distillate product is that modification liquid production process middle-molecular-weihydroxyethyl is smaller, component of highly volatile with vapor evaporation condenses one obtained again
The colorless and transparent weak solution of kind, although evaporative condenser process produces enrichment to such component, its density is 1.01-
1.04g/cm3, show that the distillate content of material is extremely low;Obviously, distillation liquid product substance is formationed, form color, it is chemical at
This aterrimus liquid has significant difference with modification liquid for point type and content etc.;Secondly, being acted as in nature to plant
Organic matter, often the smaller activity of molecular weight is bigger (macromolecular substances are generally difficult to directly be absorbed by plants), because activity at
Divide different and small molecule enrichment, distillation liquid product is superior to be modified in effect of both seedling good child-rearing and increasing crop yield
Liquid product, and have significant difference, the extremely low active high characteristic of active principle content is shown, this is opened in high-end product
Hair promotes product benefit etc. with huge advantage.
(3) production method and purposes of montanin wax resin distillate provided by the present invention are a kind of montanin waxs that would sit idle for
Resin " turning waste into wealth " it is efficient utilize new way, sufficiently excavated the potential added value of montanin wax resin, especially with
It is existing to be used cooperatively using technology (number of patent application 201610651169.2 and 201610647937.7), can veritably it accomplish
By montanin wax resin, this industrial " waste " turns waste into wealth, and eats dry bleed!The extra earning profit of relevant enterprise is increased, while
The application study for improving montanin wax resin is horizontal.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1
Montanin wax resin distillate described in the present embodiment is made by following production stage:
(1) montanin wax resin is placed in reaction kettle, by reaction promoter: reaction is added in montanin wax resin=1:3 mass ratio
Auxiliary agent carries out mechanical stirring, speed of agitator 60r/min, mixing time 20min under conditions of 70 DEG C.
(2) after the completion of step (1), by montanin wax resin: reaction is added into reaction kettle for reaction solution=1:8 mass ratio
Then liquid is stirred to react 2h, speed of agitator 80r/min under conditions of 80 DEG C, to be cooled to room temperature after reaction, stand
2h carries out solid-liquor separation.
(3) it takes out standing liquid and is centrifuged 10min under the conditions of 5000r/min, obtain supernatant, supernatant is subjected to vacuum mistake
Filter, filtered fluid are resin modified liquid stoste;By modification liquid stoste under conditions of 60 DEG C vacuum evaporation to the three of original volume
/ mono-, the condensate liquid obtained after the gas condensation being evaporated is montanin wax resin distillate, is denoted as distillate I.
The reaction promoter the preparation method comprises the following steps: pressing Tween 80: ethyl alcohol: propandiol butyl ether=1:1:3 mass ratio is by three
It is pre- to mix, mixture is obtained, the aqueous solution that mass fraction is 25% is then configured to.
The reaction solution the preparation method comprises the following steps: press sodium peroxydisulfate: sodium dichromate: acid solution=1:2:15 mass ratio will
Two kinds of salt are completely dissolved in the acid solution of heat, and wherein acid solution is the sulfuric acid containing 10% mass fraction and 4% matter
Measure the aqueous solution of the ferrous sulfate of score.
Embodiment 2
Montanin wax resin distillate described in the present embodiment is made by following production stage:
(1) montanin wax resin is placed in reaction kettle, by reaction promoter: reaction is added in montanin wax resin=1:4 mass ratio
Auxiliary agent carries out mechanical stirring, speed of agitator 55r/min, mixing time 25min under conditions of 80 DEG C.
(2) after the completion of step (1), by montanin wax resin: reaction is added into reaction kettle for reaction solution=1:12 mass ratio
Then liquid is stirred to react 2.5h, speed of agitator 90r/min under conditions of 90 DEG C, quiet to be cooled to room temperature after reaction
It sets 2h and carries out solid-liquor separation.
(3) it takes out standing liquid and is centrifuged 8min under the conditions of 4500r/min, obtain supernatant, supernatant is subjected to vacuum mistake
Filter, filtered fluid are resin modified liquid stoste;By modification liquid stoste under conditions of 60 DEG C vacuum evaporation to the three of original volume
/ mono-, the condensate liquid obtained after the gas condensation being evaporated is montanin wax resin distillate, is denoted as distillate II.
The reaction promoter the preparation method comprises the following steps: pressing Tween 80: ethyl alcohol: propandiol butyl ether=1:1.5:4 mass ratio is by three
Person mixes in advance, obtains mixture, is then configured to the aqueous solution that mass fraction is 35%.
The reaction solution the preparation method comprises the following steps: press sodium peroxydisulfate: sodium dichromate: acid solution=1:2:12 mass ratio will
Two kinds of salt are completely dissolved in the acid solution of heat, and wherein acid solution is the sulfuric acid containing 10% mass fraction and 4% matter
Measure the aqueous solution of the ferrous sulfate of score.
Embodiment 3
Montanin wax resin distillate described in the present embodiment is made by following production stage:
(1) montanin wax resin is placed in reaction kettle, by reaction promoter: montanin wax resin=1:5 mass ratio is added anti-
Auxiliary agent is answered, mechanical stirring, speed of agitator 50r/min, mixing time 30min are carried out under conditions of 90 DEG C.
(2) after the completion of step (1), by montanin wax resin: reaction is added into reaction kettle for reaction solution=1:16 mass ratio
Then liquid is stirred to react 3h, speed of agitator 100r/min under conditions of 100 DEG C, quiet to be cooled to room temperature after reaction
It sets 1.5h and carries out solid-liquor separation.
(3) it takes out standing liquid and is centrifuged 6min under the conditions of 4000r/min, obtain supernatant, supernatant is subjected to vacuum mistake
Filter, filtered fluid are resin modified liquid stoste;By modification liquid stoste under conditions of 70 DEG C vacuum evaporation to the three of original volume
/ mono-, the condensate liquid obtained after the gas condensation being evaporated is montanin wax resin distillate, is denoted as distillate III.
The reaction promoter the preparation method comprises the following steps: pressing Tween 80: ethyl alcohol: propandiol butyl ether=1:2:5 mass ratio is by three
It is pre- to mix, mixture is obtained, the aqueous solution that mass fraction is 40% is then configured to.
The reaction solution the preparation method comprises the following steps: press sodium peroxydisulfate: sodium dichromate: acid solution=1:1:10 mass ratio will
Two kinds of salt are completely dissolved in the acid solution of heat, and wherein acid solution is the sulfuric acid containing 10% mass fraction and 4% matter
Measure the aqueous solution of the ferrous sulfate of score.
The montanin wax resin distillation liquid product that 1-3 of the embodiment of the present invention is prepared is in seedling good child-rearing and increasing crop yield side
The concrete application effect in face is as follows:
One, the application effect in terms of seedling good child-rearing
1, wheat seeds sprouting is tested:
A, full seed wheat seed tap water rinse of the same size is taken, uses nothing after 10% NaClO sterilizes 10min
Bacterium distilled water flushing 7 times;The resin activated modification liquid of the montanin wax for being respectively 3% with distilled water, mass fraction, mass fraction 1%
Montanin wax resin distillate as sensitization liquid by wheat seed impregnate 6 h carry out sensitization.
B, it takes neatly to be put with batch 250, the consistent seed of sensitization to the bottom that 5 diameters are 12 cm and is covered with 1 layer of filter paper
Culture dish in, 50, every ware, each Hoagland's culture solution that 10mL is added and contains 0.75% NaCl, according to sensitization liquid difference point
It Biao Ji be not group (blank control group), IV group of modification liquid (selection best lignite wax tree of effect in terms of breeding, raising seedling
Rouge activation modification liquid IV is used as positive control, and preparation method is referring to patent CN201610647937.7), I group of distillate, distillation
II group of liquid, III group of distillate.
C, it is cultivated with constant incubator, diurnal temperature is kept at 16-26 DEG C and 10-16 DEG C, the average photoperiod
For 14 h;It fills the water the moisture that supplement evaporation loses in culture dish with weight method daily, is more than that seed is long with seed base-root length
1/ 2 standard as germination of degree after cultivating 72h, measures indices.Test result is as shown in table 1.
Application effect of the 1 montanin wax resin distillate of table in wheat seeds sprouting
Test result shows that montanin wax resin distillate and modification liquid all have one to the sprouting of wheat seed under salt stress
Fixed facilitation, and the effect of distillate is substantially better than modification liquid, the distillate of different embodiment preparations in all indexs
Sample difference on effect is little.
2, Chinese Cabbage Seeds Germination is tested:
Research object is replaced with into pakchoi seed, test method is referring to " 1, wheat seeds sprouting test ".Test result
As shown in table 2.
Application effect of the 2 montanin wax resin distillate of table in Chinese cabbage seed sprouting
Test result shows that montanin wax resin distillate and modification liquid all have the sprouting of pakchoi seed under salt stress
Certain facilitation, and the effect of distillate is substantially better than modification liquid, the distillation of different embodiment preparations in all indexs
Liquid sample difference on effect is little, this and performance of the distillate on cereal crops are much like.
3, wheat seedling growth is tested:
A, the wheat seed tap water rinse for taking full seed, with sterile distillation after 10% NaClO sterilizes 10 min
Water rinses 7 times, downward the ventral groove of seed, is neatly placed in the culture dish for being covered with sterilizing fine sand, is finally putting into illumination cultivation
Constant temperature incubation in case (set temperature is 25 DEG C, 12 h/d of light application time).Suitable deionized water is poured daily, keeps Shamian Island wet
Profit.
B, consistent sprigging will be grown into Hoagland ' s culture solution within the tenth day, and will spray the distillation of equivalent respectively
The montanin wax resin distillate that the resin activated modification liquid of the montanin wax that water, mass fraction are 3%, mass fraction are 1%, then use constant temperature
Incubator is cultivated, and 30/20 DEG C of diurnal temperature, daily illumination 16h;After culture 7 days, indices are measured.Test result is such as
Shown in table 3.
Influence of the 3 montanin wax resin distillate of table to wheat seedling growth
Test result shows that montanin wax resin distillate and modification liquid all have facilitation to the growth of wheat seedling,
And the effect of distillate is substantially better than modification liquid in all indexs, the distillate sample difference on effect of different embodiment preparations is not
Greatly.
4, pakchoi growth of seedling is tested:
Research object is replaced with into pakchoi seed, test method is referring to " 3, wheat seedling growth test ".Test result
As shown in table 4.
Influence of the 4 montanin wax resin distillate of table to pakchoi growth of seedling
Test result shows that montanin wax resin distillate and modification liquid all have the growth of pakchoi seedling under salt stress
Certain facilitation, and the effect of distillate is substantially better than modification liquid, the distillation of different embodiment preparations in all indexs
Liquid sample difference on effect is little, this and performance of the distillate on cereal crops are much like.
Two, the application effect in terms of increasing crop yield
1, wheat increase yield is tested:
A, before sowing by distilled water, mass fraction be 3% the resin activated modification liquid of montanin wax, mass fraction be 1% illiteracy
Denier wax tree rouge distillate is equably sprayed on wheat seeds respectively as seed dressing medical fluid, and routinely the sowing time is sowed after drying;Root
Distilled water group (blank control group) is respectively labeled as according to seed dressing medical fluid difference, (selection is in terms of increasing crop yield for III group of modification liquid
The resin activated modification liquid III of the best lignite wax of effect is used as positive control, and preparation method is referring to patent
CN201610647937.7), I group of distillate, II group of distillate, III group of distillate;
B, the solution identical with seed dressing medical fluid of foliage spray equivalent is distinguished since after planting second month, monthly
Until wheat maturation, during which growing environment is normal, and the disasters such as no drought and waterlogging, hot dry wind occur.Test result is as shown in table 5.
Application effect of the 5 montanin wax resin distillate of table to wheat increase yield
Test result shows that montanin wax resin distillate and modification liquid all have certain facilitation to wheat increase yield,
And the effect of distillate is substantially better than modification liquid in all indexs, the distillate sample difference on effect of different embodiment preparations is not
Greatly.
2, pakchoi simulation experiments:
Research object is replaced with into pakchoi seed, the foliage spray sample solution since after planting second week, every two weeks
The once unified harvest until the 9th week, other are referring to " 1, wheat increase yield test ".Test result is as shown in table 6.
The application effect that 6 montanin wax resin distillate of table increases production pakchoi
Test result shows that montanin wax resin distillate and modification liquid all have certain promotion to pakchoi volume increase and make
With, and the effect of distillate is substantially better than modification liquid in all indexs, the distillate sample effect of different embodiment preparations is poor
Different little, this and performance of the distillate on cereal crops are much like.
In conclusion montanin wax resin distillate all has good application effect in terms of seedling good child-rearing, increasing crop yield
Fruit;And it is substantially better than the resin activated modification liquid of the montanin wax classification product best in same field effect;Different embodiment systems
Standby distillate sample difference on effect is little;Distillate is much like in realization of both seedling good child-rearing, increasing crop yield.
Claims (4)
1. a kind of preparation method of montanin wax resin distillate, which is characterized in that specifically comprise the following steps:
(1) montanin wax resin is placed in reaction kettle, by reaction promoter: montanin wax resin=1:3-5 mass ratio is added reaction and helps
Agent stirs and evenly mixs under conditions of 70-90 DEG C;
(2) after the completion of step (1), by montanin wax resin: reaction is added into reaction kettle for reaction solution=1:8-16 mass ratio
Then liquid is stirred to react 2-3h under conditions of 80-100 DEG C, to be cooled to room temperature after reaction, it is solid to stand 1-2h progress liquid
Separation;
(3) it takes out standing liquid to be centrifuged, obtains supernatant, supernatant is subjected to vacuum filter, filtered fluid changes for resin
Property liquid stoste;By modification liquid stoste, vacuum evaporation is evaporated to the one third of original volume under conditions of 50-70 DEG C
Gas condensation after obtained condensate liquid be montanin wax resin distillate;
The reaction promoter the preparation method comprises the following steps: pressing Tween 80: ethyl alcohol: propandiol butyl ether=1:1-2:3-5 mass ratio is by three
It mixes, obtains mixture, be then configured to the aqueous solution that mass fraction is 25-40%;
Reaction solution described in step (2) the preparation method comprises the following steps: press sodium peroxydisulfate: sodium dichromate: acid solution=1:1-2:10-15
Mass ratio by two kinds of salt be completely dissolved in heat acid solution in, wherein acid solution be contain 10% mass fraction
The aqueous solution of the ferrous sulfate of sulfuric acid and 4% mass fraction.
2. the preparation method of montanin wax resin distillate according to claim 1, it is characterised in that: stirred in step (1)
Speed of agitator is 50-60r/min, mixing time 20-30min.
3. the preparation method of montanin wax resin distillate according to claim 1, it is characterised in that: stirring turns in step (2)
Speed is 80-100r/min.
4. the preparation method of montanin wax resin distillate according to claim 1, it is characterised in that: centrifugation point in step (3)
From condition are as follows: 4000-5000r/min be centrifugated 6-10min.
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Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100836524B1 (en) * | 2006-02-23 | 2008-06-12 | 한국전기연구원 | Active Material Having High Capacitance For An Electrode, Manufacturing Method thereof, Electrode And Energy Storage Apparatus Comprising The Same |
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CN106244235B (en) * | 2016-08-10 | 2017-11-10 | 昆明理工大学 | A kind of Preparation method and use of lignite wax resin modified thing |
CN106190306B (en) * | 2016-08-10 | 2017-10-13 | 云南尚呈生物科技有限公司 | A kind of resin activated modification liquid of lignite wax and its production method and purposes |
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