CN106497149B - A method of utilizing lignin prepare with scale nanometer carbon black - Google Patents
A method of utilizing lignin prepare with scale nanometer carbon black Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/50—Furnace black ; Preparation thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of methods using lignin prepare with scale nanometer carbon black, which is characterized in that including purification, oxidation, pre-reaction, condensation, washing, slurry preparation and heat treatment and etc..For the present invention using water as reaction medium, technical process is simply controllable, and particle size can be regulated and controled by above-mentioned chemical reaction and the adjusting of heat treatment high temperature carbonization technique parameter, be suitable for large-scale industrial production.And the primary partical average grain diameter of carbon black that the method for the present invention is prepared can reach 100nm hereinafter, can be applied to the fields such as reinforcing rubber, filling plastic.
Description
Technical field
The present invention relates to the preparation methods of nanometer carbon black, and in particular to a kind of to utilize lignin prepare with scale nanometer carbon black
Method, belong to productive method of chemical engineering technical field.
Background technology
Carbon black have excellent reinforcement, conduction, UV resistance, it is antistatic, dyeing etc. characteristics, be widely used in rubber, plastics,
The fields such as ink, coating.Especially in rubber industry, compared with other fillers, carbon black has apparent strengthening action and cost
Benefit advantage.Almost all of rubber product is both needed to filling carbon black, and dosage typically constitutes the 20%- of rubber product total amount
50%.And rubber industry is China's economy and the indispensable important industry of national defense construction, the carbon black consumed can account for carbon black
90% or more of total output.With the development of the social economy, the demand of carbon black will grow simultaneously with rubber industry.
Currently, China's carbon black industry can produce rubber all extraordinary carbon blacks of routine and part, but the life of China's carbon black
There are still problems with for production：(1) raw material sources and cost problem.The industrialized production generally use natural gas of carbon black, tar etc.
Non-renewable fossil resources make raw material, and burning under conditions of lack of air is made.Due to resources such as China's natural gas, oil
Deficient and coal resource is compared with horn of plenty, and domestic carbon black enterprise generally use price coal tar the cheapest is as raw material production carbon
It is black.Nonetheless, the cost of material for producing carbon black also accounts for the 80%-90% of its price.Moreover, with these non-renewable moneys
The price of the consumption in source, feedstock oil will rise steadily, further squeeze on profit space, this will bring greatly to Carbon black production enterprise
Difficulty.(2) environmental pollution and greenhouse gas emission problem.During Carbon black production, the fossil resources such as feedstock oil it is endless
Full burning can discharge the toxic and harmful gas such as a large amount of carbon monoxide, carbon dioxide, sulfur dioxide, will be further exacerbated by greenhouse effects
And environmental pollution, do not meet the economic situation of current energy-saving and emission-reduction and low-carbon.
Since above-mentioned both sides, inexpensive, environmental-friendly, nontoxic, energy large-scale industry are had in carbon black industry
The friendly process route of metaplasia production carbon black is the target that people constantly pursue.Using renewable and cheap and easy to get biomass as
Carbon source prepares Functional carbon material and just receives more and more attention.The patent of Publication No. CN102190909A discloses one kind
Obtain sugar acid solution under strong acid hydrolysis effect using biomass, colloidal carbon sphere obtained by being condensed carbonization, then through high warm at
Manage the method for obtaining nanometer carbon black.However, this method needs to make solvent using a large amount of strong acid, complex process takes, is unfavorable for
Carbon black is mass produced, and prepared black grain diameter is more than 200nm.Bioblast can be prepared on a large scale about using lignin
Carbon black particle of the seed diameter less than 100nm temporarily has no document and patent report.
Invention content
It is an object of the invention to for the above-mentioned prior art the problem of, provide it is a kind of using lignin it is extensive
The method for preparing carbon black of the primary grain size less than 100nm.
To achieve the above object, technical solution provided by the invention is as follows：
A method of preparing nanometer carbon black using lignin, which is characterized in that include the following steps：
(1) it purifies：100g lignin stock dispersions are obtained into lignin dispersion liquid in water, are adjusted with sodium hydroxide or hydrochloric acid
The pH value of the lignin dispersion liquid be 9-13, after mechanical agitation makes lignin fully dissolve, using centrifugation, suction filtration, press filtration or
The mode of ultrafiltration detaches cellulose, hemicellulose and insoluble impurity in removal lignin liquor, the lignin liquor after must purifying.
(2) it aoxidizes：The pH value of lignin liquor after purification is adjusted to 6-12,1-20g hydrogen peroxide is then added, adds
Heat is stirred to react 10-120 minutes to 45-70 DEG C, the lignin liquor after must aoxidizing.
(3) pre-reaction：The pH value for adjusting the lignin liquor after oxidation is 8-13, and is warming up to 50-85 DEG C, is added and is modified
Agent 1-50g reacts 0.5-12 hours, obtains modified lignin liquor.
(4) it is condensed：The modified lignin liquor pH value that step (3) obtains is adjusted to 9-13, and controls temperature and exists
80-92 DEG C, condensation reaction 0.5-5 hours obtains lignin colloid solution.Lignin colloid ball in gained lignin colloid solution
Average grain diameter be 50-500nm.
(5) it washs：The pH value for the lignin colloid solution that step (4) is obtained is adjusted to 2-3, and it is 80- to keep temperature
It 90 DEG C, filters and washes 3-5 times after solution lignin caking, to remove unreacted soluble small molecular, must be modified wooden
Element.
(6) slurry preparation：The modified lignin resin that washing is obtained and the slurry that water mixed preparing solid content is 10-50%,
And the pH value for adjusting slurry is 6-12.
(7) it is heat-treated：The slurry that step (6) is obtained sprayed into 1200-2100 DEG C with 1-200L/ hours spray velocitys
In ullrasonic spraying pyrolysis furnace or carbon black reacting furnace, it is used in combination bag hose to collect superfine carbon black flue dust, obtains nanometer carbon black.Gained nanometer
Carbon black primary partical average grain diameter is 20-80nm.
By said program, it is preferable that the lignin described in step (1) is the pair in paper industry and bio-ethanol industry
Product, such as alkali lignin, sulphite lignin, sodium lignin sulfonate, calcium lignosulfonate, magnesium lignosulfonate or enzymolysis wood
One or more of quality mixture.
By said program, it is preferable that in step (2), the pH value of the lignin liquor after purification is adjusted to 6-12 when institutes
PH adjusting agent is the sulfuric acid of a concentration of 0.1%-5%；In step (3), the pH value of the lignin liquor after oxidation is adjusted
For 8-13 when pH adjusting agent used be sodium hydroxide；When modified lignin liquor pH value being adjusted to 9-13 in step (4)
PH adjusting agent used is hydrochloric acid or sodium hydroxide；It is used when adjusting lignin colloid solution ph to 2-3 in step (5)
The dilute sulfuric acid that pH adjusting agent is 2%.
By said program, it is preferable that described in step (6) adjust slurry pH value the specific steps are：Use sodium hydroxide
The pH value of slurry is adjusted to 10.5-12；Alternatively, first adjusting the pH value of slurry to 10.5 or more, then with hydrochloric acid tune with sodium hydroxide
The pH value of slurry is saved to 6-10.5.
By said program, it is preferable that in step (3), the modifying agent be only aldehydes modifying agent or aldehydes modifying agent with
Phenol-modified dose of mixture；Further include that 1~30g of epoxies modifying agent is added it is highly preferred that in step (4) when condensation reaction
The step of.
By said program, it is preferable that in step (3), the modifying agent is epoxies modifying agent, is condensed in step (4) anti-
At once, further include the steps that 1~30g of aldehydes modifying agent is added.
By said program, it is preferable that the aldehydes modifying agent is formaldehyde, glyoxal, one kind in glutaraldehyde or two
Kind or more mixture.
By said program, it is preferable that described phenol-modified dose is phenol, hydroquinone, bisphenol-A, water soluble phenol resin
In any one or more mixture.
By said program, it is preferable that it is sweet that the epoxies modifying agent is bisphenol A diglycidyl ether, resorcinol shrinks
The mixing of one or more of oily ether, ethylene glycol diglycidylether, Polyethylene Glycol Bisglycidyl Ether, epoxychloropropane
Object.
The reaction principle of the present invention is as follows：
By oxidation reaction, lignin molecule amount is reduced, then increase in lignin molecule and can be condensed by pre-reaction
The functional group content of reaction so that lignin molecule forms more uniform nanometer ball-type glue in subsequent condensation reaction
Body avoids lacking reactivity lignin molecule fragment residual, to weaken the fusion phenomenon of lignin particle, reaches regulation and control wood
The purpose of quality size and product nano black grain diameter and structure.
Compared with the prior art, the beneficial effects of the invention are as follows：
1, compared with traditional carbon black industrialized preparing process, lignin raw material itself used in the present invention belongs to solid
Waste, it is cheap and easy to get and renewable.
2, the present invention make lignin conversion be carbon black, cost of material compared with prior art preparation carbon black cost of material at least
30% is reduced, there is larger price advantage.
3, compared with preparing the method for carbon black using other biomass, carbon black that the present invention is prepared using lignin
Primary partical average grain diameter can reach 100nm hereinafter, can be applied to reinforcing rubber, filling plastic etc..
4, the present invention uses water as reaction medium, and technical process is simply controllable, and particle size can pass through above-mentioned chemistry
Reaction regulates and controls with the adjusting of high temperature cabonization technological parameter, is suitable for large-scale industrial production.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
(1) it purifies：100g alkali lignins are scattered in 400g water, addition sodium hydrate regulator solution pH value to 12 and machine
Tool stirs.After alkali lignin fully dissolves, cellulose and insoluble impurity in removal lignin liquor are detached using suction filtration mode,
Lignin liquor after must purifying.
(2) it aoxidizes：The pH value that the lignin liquor after purification is adjusted with a concentration of 1% sulfuric acid is 6.5, is then added
16g hydrogen peroxide is heated to 55 DEG C and stirs oxidation reaction 1 hour, the lignin liquor after must aoxidizing.
(3) pre-reaction：The pH value that the lignin liquor after oxidation is adjusted with NaOH is 10, and is warming up to 65 DEG C, and ring is added
Oxygen chloropropane 25g reacts 3 hours, obtains modified lignin liquor.
(4) it is condensed：Modified lignin liquor pH value is adjusted to 12 with NaOH, and is warming up to 90 DEG C and adds formaldehyde again
20g, condensation reaction 1 hour, obtains lignin colloid solution.Through measuring the lignin colloid solution using dynamic light scattering technique
The average grain diameter of middle lignin colloid ball is 180nm.
(5) it washs：The pH value of the lignin colloid solution obtained with 2% sulfuric acid solution regulating step (4) is protected to 2.7
It is 85 DEG C to hold temperature, filters and washes 5 times after caking occurs in solution, to remove unreacted soluble small molecular, obtains modification
Lignin.
(6) slurry preparation：The slurry that the modified lignin resin that step (5) is obtained is 20% with water mixed preparing solid content,
It is 12 to be used in combination sodium hydroxide to adjust the pH value of slurry.
(7) it is heat-treated：By slurry made from step (6) with the ullrasonic spraying of 1200 DEG C of spray velocity penetrating in 1L/ hours
In pyrolysis furnace, slurry is instantaneously carbonized, and collects superfine carbon black flue dust with bag hose, obtains carbon black.
It presses《The indirect determination reflectivity method of GB/T 3781.17-2008 carbon blacks-grain size》It measures and is received made from the present embodiment
Rice carbon black primary partical average grain diameter is 70nm.
Embodiment 2
(1) it purifies：100g alkali lignins are scattered in 400g water, simultaneously machinery stirs addition sodium hydroxide adjusting pH value to 12
It mixes.After alkali lignin fully dissolves, cellulose and insoluble impurity in removal lignin liquor are detached using suction filtration mode, must be carried
Lignin liquor after pure.
(2) it aoxidizes：The pH value that the lignin liquor after purification is adjusted with a concentration of 1% sulfuric acid is 9, and 5g mistakes are then added
Hydrogen oxide, heating stirring under the conditions of 60 DEG C aoxidize 30 minutes.
(3) pre-reaction：The pH value that the lignin liquor after oxidation is adjusted with NaOH is 9, and is warming up to 80 DEG C, and phenol is added
2g, formaldehyde 20g react 2 hours, obtain modified lignin liquor.
(4) it is condensed：Modified lignin liquor pH value is adjusted to 12, and at a temperature of 92 DEG C with NaOH, condensation reaction 1
Hour, then add epoxychloropropane 5g, the reaction was continued 0.5 hour, obtains lignin colloid solution.After measured, the lignin colloid
The average grain diameter of lignin colloid ball is 134nm in solution.
(5) it washs：With the lignin colloid solution ph in 2% sulfuric acid solution regulating step 4 to 2.5, and keep temperature
It is 85 DEG C, filters and wash 5 times after luming, to remove unreacted soluble small molecular, obtain modified lignin resin.
(6) slurry preparation：The slurry that the modified lignin resin that step (5) is obtained is 25% with water mixed preparing solid content,
It is 12 to be used in combination sodium hydroxide to adjust the pH value of slurry.
(7) it is heat-treated：Slurry made from step (6) is anti-with the carbon black of 1800 DEG C of spray velocity penetrating in 200L/ hours
It answers in stove, slurry is instantaneously carbonized, and collects superfine carbon black flue dust with bag hose, obtains carbon black.
After measured, the nanometer carbon black primary partical average grain diameter that the present embodiment is prepared is 21nm.
Embodiment 3
(1) it purifies：100g sodium lignin sulfonates are scattered in 400g water, addition sodium hydroxide adjusting pH value to 11 and machine
Tool stirs.After sodium lignin sulfonate fully dissolves, cellulose in lignin liquor and not is separated off using suction filtration mode
Molten impurity, the lignin liquor after must purifying.
(2) it aoxidizes：The pH value that the lignin liquor after purification is adjusted with a concentration of 1% sulfuric acid is 6.5, and 5g is then added
Hydrogen peroxide, heating stirring under the conditions of 55 DEG C aoxidize 60 minutes.
(3) pre-reaction：The pH value that the lignin liquor after oxidation is adjusted with NaOH is 12, and is warming up to 55 DEG C, between addition
Benzenediol glycidol ether 2g, formaldehyde 18g react 3 hours, obtain modified lignin liquor.
(4) it is condensed：Modified lignin liquor pH value is adjusted to 12, and at a temperature of 92 DEG C with NaOH, condensation reaction 1
Hour, lignin colloid solution is obtained, after measured, the average grain diameter of lignin colloid ball is in the lignin colloid solution
87nm。
(5) it washs：With the lignin colloid solution ph in 2% sulfuric acid solution regulating step 4 to 3, and the temperature is kept to be
It 90 DEG C, filters and washes 3 times after luming, to remove unreacted soluble small molecular, obtain modified lignin resin.
(6) slurry preparation：The slurry that the modified lignin resin that step (5) is obtained is 25% with water mixed preparing solid content,
It is 12 to be used in combination sodium hydroxide to adjust the pH value of slurry.
(7) it is heat-treated：The carbon black that the slurry that step (6) is obtained sprays into 1800 DEG C with 10L/ hours spray velocitys reacts
In stove, slurry is instantaneously carbonized, and collects superfine carbon black flue dust with bag hose, obtains carbon black.
After measured, the nanometer carbon black primary partical average grain diameter that the present embodiment is prepared is 19nm.
Embodiment 4
(1) it purifies：100g calcium lignosulfonates are scattered in 400g water, addition sodium hydroxide adjusting pH value to 11 and machine
Tool stirs.After calcium lignosulfonate fully dissolves, cellulose in lignin liquor and not is separated using suction filtration mode
Molten impurity, the lignin liquor after must purifying.
(2) it aoxidizes：The pH value that the lignin liquor after purification is adjusted with a concentration of 1% sulfuric acid is 9.5, is then added
12g hydrogen peroxide, heating stirring under the conditions of 50 DEG C aoxidize 60 minutes.
(3) pre-reaction：The pH value that the lignin liquor after oxidation is adjusted with NaOH is 10.5, and is warming up to 80 DEG C, is added
Water soluble phenol resin 5g, formaldehyde 15g react 3 hours, obtain modified lignin liquor.
(4) it is condensed：Modified lignin liquor pH value is adjusted to 12, and at a temperature of 90 DEG C with NaOH, condensation reaction
0.5 hour, obtained lignin colloid solution, after measured, the average grain diameter of lignin colloid ball in the lignin colloid solution
For 134nm.
(5) it washs：With the lignin colloid solution ph in 2% sulfuric acid solution regulating step 4 to 3, and the temperature is kept to be
It 90 DEG C, filters and washes 5 times after luming, to remove unreacted soluble small molecular, obtain modified lignin resin.
(6) slurry preparation：The slurry that the modified lignin resin that step (5) is obtained is 20% with water mixed preparing solid content,
And it is again 7 with the pH value of hydrochloric acid adjusting slurry that the pH value that slurry is first adjusted with sodium hydroxide, which is 12,.
(7) it is heat-treated：The slurry that step (6) is obtained sprays into 1200 DEG C of ullrasonic spraying with 5L/ hours spray velocitys
In pyrolysis furnace, slurry is instantaneously carbonized, and collects superfine carbon black flue dust with bag hose, obtains carbon black.
After measured, the nanometer carbon black primary partical average grain diameter that the present embodiment is prepared is 36nm.
Embodiment 5
(1) it purifies：100g alkali lignins are scattered in 400g water, simultaneously machinery stirs addition sodium hydroxide adjusting pH value to 12
It mixes.After alkali lignin fully dissolves, cellulose and insoluble impurity in lignin liquor are separated off using suction filtration mode, obtained
Lignin liquor after purification.
(2) it aoxidizes：10g hydrogen peroxide, heating stirring under the conditions of 55 DEG C, oxygen are added into the lignin liquor after purification
Change 60 minutes.
(3) pre-reaction：The pH value that the lignin liquor after oxidation is adjusted with NaOH is 12, and is warming up to 65 DEG C, and benzene is added
Phenol 5g, formaldehyde 19g react 3 hours, obtain modified lignin liquor.
(4) it is condensed：Modified lignin liquor pH value is adjusted to 12, and at a temperature of 90 DEG C, condensation reaction 1 hour,
Lignin colloid solution is obtained, after measured, the average grain diameter of lignin colloid ball is 90nm in the lignin colloid solution.
(5) it washs：With the lignin colloid solution ph in 2% sulfuric acid solution regulating step 4 to 2.5, and keep temperature
It is 85 DEG C, filters and wash 5 times after luming, to remove unreacted soluble small molecular, obtain modified lignin resin.
(6) slurry preparation：The slurry that the modified lignin resin that step (5) is obtained is 25% with water mixed preparing solid content,
The pH value of slurry is adjusted to 12 with sodium hydroxide.
(7) it is heat-treated：The carbon black that the slurry that step (6) is obtained sprays into 1900 DEG C with 100L/ hours spray velocitys is anti-
It answers in stove, slurry is instantaneously carbonized, and collects superfine carbon black flue dust with bag hose, obtains carbon black.
After measured, the nanometer carbon black primary partical average grain diameter that the present embodiment is prepared is 24nm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (9)
1. a kind of method preparing nanometer carbon black using lignin, which is characterized in that include the following steps：
(1) it purifies：100g lignin stock dispersions are obtained into lignin dispersion liquid in water, are purified, the lignin after must purifying is molten
Liquid；
(2) it aoxidizes：The pH value of lignin liquor after purification is adjusted to 6-12,1-20g hydrogen peroxide is then added, is heated to
45-70 DEG C is stirred to react 10-120 minutes, the lignin liquor after must aoxidizing；
(3) pre-reaction：The pH value for adjusting the lignin liquor after oxidation is 8-13, and is warming up to 50-85 DEG C, and modifying agent 1- is added
50g reacts 0.5-12 hours, obtains modified lignin liquor；The modifying agent is that only aldehydes modifying agent or aldehydes are modified
Mixture or epoxies modifying agent of the agent with phenol-modified dose；
(4) it is condensed：The pH value for the modified lignin liquor that step (3) is obtained is adjusted to 9-13, and controls temperature in 80-
92 DEG C, condensation reaction 0.5-5 hours obtains lignin colloid solution；
(5) it washs：The pH value for the lignin colloid solution that step (4) is obtained is adjusted to 2-3, and it is 80-90 DEG C to keep temperature,
It filters and washes after lignin caking in solution, obtain modified lignin resin；
(6) slurry preparation：The modified lignin resin that washing obtains in step (5) is mixed with water, it is 10-50% to be configured to solid content
Slurry, and adjust slurry pH value be 6-12；
(7) it is heat-treated：The slurry that step (6) is obtained sprays into 1200-2100 DEG C of ultrasound with 1-200L/ hours spray velocitys
It sprays in pyrolysis furnace or carbon black reacting furnace, obtains nanometer carbon black；The primary partical average grain diameter of the nanometer carbon black be 100nm with
Under.
2. the method according to claim 1 for preparing nanometer carbon black using lignin, which is characterized in that institute in step (1)
Stating method of purification is specially：The pH value that the lignin dispersion liquid is adjusted with sodium hydroxide or hydrochloric acid is 9-13, and stirring makes wooden
After plain fully dissolving, centrifugation, suction filtration, press filtration or ultrafiltration.
3. the method according to claim 1 for preparing nanometer carbon black using lignin, which is characterized in that institute in step (1)
The lignin stated be alkali lignin, sulphite lignin, sodium lignin sulfonate, calcium lignosulfonate, magnesium lignosulfonate or
One or more of enzymolysis xylogen mixture.
4. the method according to claim 1 for preparing nanometer carbon black using lignin, which is characterized in that
In step (2), pH adjusting agent used is a concentration of when the pH value of the lignin liquor after purification is adjusted to 6-12
The sulfuric acid of 0.1%-5%；
In step (3), pH adjusting agent used is sodium hydroxide when the pH value of the lignin liquor after oxidation is adjusted to 8-13；
PH adjusting agent used is hydrochloric acid or hydroxide when adjusting modified lignin liquor pH value to 9-13 in step (4)
Sodium；
The dilute sulfuric acid that pH adjusting agent used is 2% when adjusting lignin colloid solution ph to 2-3 in step (5).
5. the method according to claim 4 for preparing nanometer carbon black using lignin, which is characterized in that institute in step (6)
State adjust slurry pH value the specific steps are：
The pH value of slurry is adjusted to 10.5-12 with sodium hydroxide；Alternatively,
The pH value that slurry is first adjusted with sodium hydroxide adjusts the pH value of slurry to 6-10.5 to 10.5 or more, then with hydrochloric acid.
6. the method according to claim 1 for preparing nanometer carbon black using lignin, which is characterized in that in step (3), institute
Modifying agent is stated as only aldehydes modifying agent or aldehydes modifying agent and phenol-modified dose of mixture, wherein the aldehydes modifying agent
For the mixture of one or more of formaldehyde, glyoxal, glutaraldehyde, described phenol-modified dose be phenol, hydroquinone,
Any one or more mixture in bisphenol-A, water soluble phenol resin.
7. the method for preparing nanometer carbon black using lignin stated according to claim 6, which is characterized in that condensation in step (4)
Further include the steps that 1~30g of epoxies modifying agent is added when reaction.
8. the method according to claim 1 for preparing nanometer carbon black using lignin, which is characterized in that in step (3), institute
It is epoxies modifying agent to state modifying agent, and in step (4) when condensation reaction, further includes the step that 1~30g of aldehydes modifying agent is added
Suddenly；Wherein, the aldehydes modifying agent is the mixture of one or more of formaldehyde, glyoxal, glutaraldehyde.
9. the method according to claim 7 or 8 for preparing nanometer carbon black using lignin, which is characterized in that the epoxy
Class modifying agent is bisphenol A diglycidyl ether, resorcinol glycidol ether, ethylene glycol diglycidylether, polyethylene glycol contracting
The mixture of one or more of water glycerin ether, epoxychloropropane.
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| EP3894483A4 (en) * | 2018-12-14 | 2022-09-21 | Ray W. Chrisman | Carbon black from biomass |
| CN111777877A (en) * | 2020-06-19 | 2020-10-16 | 茂名环星新材料股份有限公司 | Low-loss air preheater heat exchange method |
| CN116333516B (en) * | 2023-02-27 | 2024-03-08 | 吉林大学 | Preparation method of lignin-based nano carbon black |
| CN117487396A (en) * | 2023-11-03 | 2024-02-02 | 鹤山市炎墨科技有限公司 | Black solder resist ink and preparation method and application thereof |
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| CN104310376B (en) * | 2014-10-10 | 2016-05-18 | 江苏省特种设备安全监督检验研究院无锡分院 | A kind of post processing cross-linking method of biomass carbon source material hydrothermal carbonization spherical particles |
| CN104576077A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Graphene/ lignin-based activated carbon preparation method and application in supercapacitors |
| CN105293488B (en) * | 2015-10-23 | 2017-07-21 | 北京林业大学 | Lignin-Based Activated Carbon microballoon, its preparation method and application |
| CN105399872B (en) * | 2015-12-22 | 2018-06-15 | 齐鲁工业大学 | A kind of method and application using Jujun grasses Preparation of Activated Carbon with Lignin |
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