CN109293462B - Passivation method of nickel hydrazine nitrate - Google Patents
Passivation method of nickel hydrazine nitrate Download PDFInfo
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- CN109293462B CN109293462B CN201811322688.XA CN201811322688A CN109293462B CN 109293462 B CN109293462 B CN 109293462B CN 201811322688 A CN201811322688 A CN 201811322688A CN 109293462 B CN109293462 B CN 109293462B
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- nickel
- coating agent
- hydrazine nitrate
- nitrate
- hydrazine
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- LNAWIXGXVIGLOJ-UHFFFAOYSA-N hydrazine nickel(2+) dinitrate Chemical compound [N+](=O)([O-])[O-].NN.[Ni+2].[N+](=O)([O-])[O-] LNAWIXGXVIGLOJ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000002161 passivation Methods 0.000 title claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000012188 paraffin wax Substances 0.000 claims description 15
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 14
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- -1 hydrazino nickel nitrate Chemical compound 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 5
- 238000012216 screening Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 20
- 238000005474 detonation Methods 0.000 description 12
- 229920002635 polyurethane Polymers 0.000 description 11
- 239000004814 polyurethane Substances 0.000 description 11
- 238000010304 firing Methods 0.000 description 8
- 230000000977 initiatory effect Effects 0.000 description 6
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
- C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a passivation method of nickel hydrazine nitrate, which comprises the steps of putting a coating agent into a solvent and stirring to obtain a coating agent solution or dispersion liquid; weighing hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into the coating agent solution or dispersion liquid, and stirring at constant temperature to obtain a mixed solution; and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at a certain temperature to remove the solvent until no fraction is evaporated out to obtain the coated nickel hydrazine nitrate. The passivation method has the advantages of wide application range, good coating effect, widening of the application range of the coating agent, convenience in screening the coating agent, simplicity in operation, lower cost and suitability for large-scale production.
Description
Technical Field
The application relates to a passivation method of pyrotechnic compositions, in particular to a passivation method of nickel hydrazine nitrate.
Background
Nickel hydrazine nitrate belongs to a complex primary explosive and has the characteristics of simple manufacturing process, good product performance and stable quality. However, the detonation pressure is usually less than 80MPa, which indicates that the nickel hydrazine nitrate sample has high sensitivity, is easy to combust or explode in the processes of preparation, storage, transportation and the like, has high potential safety hazard, and therefore needs to be passivated.
Patent CN88101549A discloses a passivation mode of nickel hydrazine nitrate, and it adopts graphite colloid and nickel hydrazine nitrate to disperse, has reduced the friction between the nickel hydrazine nitrate through the lubricity performance of graphite, has played the passivation effect. However, the graphite particles are only spaced among the nickel hydrazine nitrate particles, so that the collision probability among the nickel hydrazine nitrate particles is reduced, and the isolation among the nickel hydrazine nitrate particles cannot be completely realized. Zhouweiwei et al (bulletin of explosives and powders, volume 38, phase 5) disclose that hydrazine nickel nitrate is coated inaccurately with an aqueous polyurethane emulsion by emulsion breaking, which allows the detonation pressure value of hydrazine nickel nitrate to be 383MPa and the 50% firing distance to be 80% or more of that of uncoated nickel nitrate. The method realizes the complete physical isolation of the nickel hydrazine nitrate particles, and improves the safety of the nickel hydrazine nitrate in the processes of preparation, storage, transportation and the like. However, the method has complex steps of emulsification before demulsification, requires the coating reagent to have emulsification, needs fine control in the demulsification and precipitation process, greatly reduces the selection of the coating reagent, has narrow application range, cannot realize good coating of part of nickel hydrazine nitrate particles in the complex demulsification and precipitation process, introduces impurities into the coated nickel hydrazine nitrate particles due to the addition of the demulsifier, and increases the cost due to the fact that part of the coating reagent is left in the solution. Therefore, there is a need to develop a passivation method with wider application range and better coating effect.
Disclosure of Invention
The application provides a hydrazine nickel nitrate passivation method which is wide in application range and good in coating effect, and the specific scheme is as follows:
(1) putting a certain amount of coating agent into a solvent, and ultrasonically stirring at a constant temperature of 30-70 ℃ until the coating agent is completely dissolved or dispersed to obtain a coating agent solution or dispersion liquid;
(2) weighing a certain amount of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into the coating agent solution or dispersion liquid, wherein the ratio of the hydrazine nitrate nickel powder to the coating agent solution or dispersion liquid is 5 g: 15-50mL, and stirring at constant temperature of 30-70 ℃ for 0.5-2h to obtain a mixed solution;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at the temperature of 30-60 ℃ to remove the solvent until no fraction is evaporated out to obtain the coated nickel hydrazine nitrate.
Preferably, in the step (1), the coating agent is paraffin, the solvent is ethyl acetate, and 5-20wt% paraffin solution is prepared; in step (3), the temperature at which the vacuum rotary distillation was carried out was 45 ℃.
Preferably, in the step (1), the coating agent is graphite and phenolic resin, the mass ratio of the phenolic resin to the graphite is 2:8, the solvent is alcohol, and 5-20wt% of graphite dispersion liquid is prepared; in step (3), the temperature at which the vacuum rotary distillation was carried out was 60 ℃.
Preferably, in the step (2), after the hydrazine nitrate nickel powder is added, ethylenediamine is added, and the ratio of ethylenediamine to the hydrazine nitrate nickel powder is 5-20 μ L: 5g of the total weight.
The beneficial effect of this application:
(1) the application range of the coating agent is widened by a vacuum rotary distillation method, the coating agents with various performances can be conveniently screened, and inorganic substances can be used as the components of the coating agent, so that the passivation mode has a wide application range.
(2) The solvent is evaporated by a vacuum rotary distillation method, and the solute is completely remained on the surface of the nickel hydrazine nitrate particles, so that the coating agent can be ensured to completely coat the nickel hydrazine nitrate particles, and the safety of the nickel hydrazine nitrate is improved.
(3) The sharp corners or edges of the surface of the nickel hydrazine nitrate particles are passivated by the complexing agent ethylenediamine, so that the safety of the nickel hydrazine nitrate is further improved.
(4) The method is simple to operate, low in cost and suitable for large-scale production.
Detailed Description
Example 1
(1) Putting a certain amount of paraffin into ethyl acetate, and ultrasonically stirring at a constant temperature of 65 ℃ until the paraffin is completely dissolved to obtain an ethyl acetate solution of 15wt% of paraffin;
(2) weighing 5g of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into 25mL of coating agent solution, and stirring at the constant temperature of 65 ℃ for 1h to obtain mixed solution;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at 45 ℃ to remove the solvent until no fraction is evaporated out to obtain paraffin-coated nickel hydrazine nitrate.
Example 2
(1) Putting a certain amount of graphite and phenolic resin into alcohol, wherein the mass ratio of the phenolic resin to the graphite is 2:8, and ultrasonically stirring at a constant temperature of 30 ℃ until the graphite is completely dispersed to obtain an alcohol dispersion liquid of graphite with the weight percent of 15;
(2) weighing 5g of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into 25mL of coating agent dispersion liquid, and stirring the mixture at constant temperature of 30 ℃ for 1h to obtain mixed liquid;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at the temperature of 30 ℃ to remove the solvent until no fraction is distilled out, thereby obtaining the graphite-coated nickel hydrazine nitrate.
Example 3
(1) Putting a certain amount of sodium stearate into distilled water, and ultrasonically stirring at a constant temperature of 45 ℃ until the sodium stearate is completely dissolved to obtain 15wt% of distilled water solution of the sodium stearate;
(2) weighing 5g of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into 25mL of coating agent solution, and stirring at the constant temperature of 45 ℃ for 1h to obtain mixed solution;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at the temperature of 60 ℃ to remove the solvent until no fraction is distilled out to obtain the sodium stearate-coated nickel hydrazine nitrate.
Example 4
(1) Putting a certain amount of waterborne polyurethane into distilled water, and ultrasonically stirring at a constant temperature of 45 ℃ until the waterborne polyurethane is completely dissolved to obtain a distilled water solution of 15wt% of waterborne polyurethane;
(2) weighing 5g of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into 25mL of coating agent solution, and stirring at the constant temperature of 45 ℃ for 1h to obtain mixed solution;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at the temperature of 60 ℃ to remove the solvent until no fraction is evaporated out to obtain the aqueous polyurethane-coated nickel hydrazine nitrate.
Example 5
The procedure was as in the preparation of example 1, except that a 20wt% paraffin solution in ethyl acetate was prepared in step (1).
Example 6
The procedure was as in the preparation of example 1, except that a 10wt% paraffin solution in ethyl acetate was prepared in step (1).
Example 7
The same procedure as in example 1 was followed, except that 0.1. mu.L of ethylenediamine was added in step (2).
Example 8
The same procedure as in example 1 was followed, except that 10. mu.L of ethylenediamine was added in step (2).
Example 9
The same procedure as in example 1 was followed, except that 100. mu.L of ethylenediamine was added in step (2).
The initiation pressure and 50% firing distance were measured for the above examples by reference to the GJB772A-97 standard method, and the results are shown in Table 1:
TABLE 1
Sample (I) | Detonation pressure (MPa) | 50% distance fired (cm) |
Uncoated nickel hydrazine nitrate | 56 | 2.44 |
Example 1 | 403 | 2.01 |
Example 2 | 345 | 2.40 |
Example 3 | 320 | 1.89 |
Example 4 | 352 | 2.00 |
Practice ofExample 5 | 482 | 1.83 |
Example 6 | 280 | 2.23 |
Example 7 | 410 | 2.01 |
Example 8 | 443 | 2.00 |
Example 9 | 464 | 1.91 |
Through examples 1-4, it can be found that the passivation method of the present application can adopt a wide range of coating agents, not only can adopt the waterborne polyurethane in the prior art, but also can adopt other paraffin, sodium stearate and graphite with lubricating property, and especially can adopt inorganic lubricant graphite for coating, so that the passivation method of the present application is not limited to organic substances but also can be widened to inorganic substances when screening the coating agents. Because graphite does not have good coating capacity, the application adopts phenolic resin as a binder to coat the graphite on the surface of the nickel hydrazine nitrate through vacuum rotary evaporation. Compared with the demulsification method in the prior art, the passivation method disclosed by the application example 4 can find that the detonation pressure of 352MPa can be achieved by adopting 15wt% of waterborne polyurethane, the detonation pressure is obviously higher than 225MPa of 16wt% of waterborne polyurethane adopted by the demulsification method, even higher than 310MPa of 32wt% of waterborne polyurethane, although the detonation pressure is lower than 383MPa of the optimized demulsification method, the consumption of waterborne polyurethane in the example 4 is less, and if the same consumption of waterborne polyurethane is achieved by the demulsification method, the passivation method disclosed by the application can achieve higher detonation pressure. The comparison further shows that the demulsification method has complex process and difficult control, part of the coating agent is dissolved in water and can not be coated, and part of nickel hydrazine nitrate is not coated in the demulsification and precipitation process. Through comparison of examples 1-4, it can be found that the screening of the corresponding coating agent is convenient, the detonation pressure and 50% firing distance of different coating agents are different due to different properties of the coating agents, the paraffin coating has the highest detonation pressure, and the 50% firing distance of the graphite coating is reduced to the minimum, which is probably related to the coated hydrazine nitrate nickel particles which have better organic substance film-forming property and can be attached, the graphite has a certain shape, the attachment degree of the surface of the hydrazine nitrate nickel particles is relatively low, and the lubricity of the coating agent and the hot melting (heat absorption capacity) of the coating agent can also influence the detonation pressure and the 50% firing distance. The highest initiation pressure of the paraffin serving as the coating agent is probably related to good film forming property of the coating agent, and the film forming is uniform, so that the 50% ignition distance of the coating agent still reaches 82% of that of uncoated fireworks and crackers, and the coating agent can still be applied to the field of fireworks and crackers. The graphite used as the coating agent has a higher 50% ignition distance which is probably related to the relatively lower degree of fit between the graphite and the nickel hydrazine nitrate particles, and can realize higher initiation pressure through the lubricating action. The screening shows that the paraffin and graphite are adopted as the coating agent to obtain better effect.
It can be seen from a comparison of examples 1,5 and 6 that the more paraffin wax is used, the thicker the particles coated with the nickel hydrazine nitrate particle layer, the higher the initiation pressure and the lower the 50% firing distance. This indicates that the cladding method, while increasing the detonation pressure, would result in a corresponding 50% reduction in firing distance. Since the nickel hydrazine nitrate particles are caused to detonate by friction, the friction involved with sharp corners or edges of the nickel hydrazine nitrate particles is more easily generated, and the friction between opposite faces generates more heat, and even if the nickel hydrazine nitrate is coated, the possibility that the sharp corners or edges break through the coating is easier than other positions. On the basis of the cognition, the applicant adopts the competition of trace complexing agent and hydrazine for nickel ions according to the characteristics of the nickel hydrazine nitrate, so that sharp corners or edges of nickel hydrazine nitrate particles are passivated, the difficulty degree of the nickel hydrazine nitrate particles breaking through the coating is further increased, and the friction probability and the heat generated by friction are reduced. It can be seen from comparison of examples 1,7-9 that when 0.1 μ L of ethylenediamine was added, the initiation pressure was slightly increased due to the reduction of a small number of sharp corners or edges, and there was a very slight loss of nickel hydrazine nitrate, but there was almost no change as a whole, so that the 50% firing distance was not decreased relative to example 1. When the addition amount of ethylenediamine is further increased to 10 mu L, the detonation pressure is greatly increased, and the 50% ignition distance is only slightly reduced, which shows that most or all sharp corners or edges of nickel hydrazine nitrate particles are passivated, nickel ions at the positions react with the ethylenediamine to dissolve so that the sharp portions are not located and only the passivated portions are left, and nickel hydrazine nitrate has trace loss but does not influence the whole. However, when the addition amount of ethylenediamine is 100 muL, the ethylenediamine affects the hydrazine nickel nitrate on the whole, so that the 50% ignition distance of the hydrazine nickel nitrate is obviously reduced, and the initiation pressure of the hydrazine nickel nitrate is further increased due to the reduction of the content of the hydrazine nickel nitrate. According to the results, the proportion of ethylenediamine to the hydrazine nitrate nickel powder is 5-20 muL: 5g is most suitable.
The present invention is not limited to the above embodiments, and any other products in various forms can be obtained by the teaching of the present invention, but any changes in the shape or structure thereof, which are the same as or similar to the technical solutions of the present invention, fall within the protection scope of the present invention.
Claims (3)
1. A passivation method of nickel hydrazine nitrate is characterized by comprising the following steps:
(1) putting a certain amount of coating agent into a solvent, and ultrasonically stirring at a constant temperature of 30-70 ℃ until the coating agent is completely dissolved or dispersed to obtain a coating agent solution or dispersion liquid;
(2) weighing a certain amount of hydrazine nitrate nickel powder, slowly adding the hydrazine nitrate nickel powder into the coating agent solution or dispersion liquid, and then adding ethylenediamine, wherein the ratio of the ethylenediamine to the hydrazine nitrate nickel powder is 5-20 mu L: 5g, the proportion of the hydrazine nitrate nickel powder to the coating agent solution or dispersion is 5 g: 15-50mL, and stirring at constant temperature of 30-70 ℃ for 0.5-2h to obtain a mixed solution;
(3) and (3) placing the mixed solution into a single-neck flask, and performing vacuum rotary distillation at the temperature of 30-60 ℃ to remove the solvent until no fraction is evaporated out to obtain the coated nickel hydrazine nitrate.
2. The passivation method of nickel hydrazine nitrate according to claim 1, characterized in that in the step (1), the coating agent is paraffin, the solvent is ethyl acetate, and a 5-20wt% paraffin solution is prepared; in step (3), the temperature at which the vacuum rotary distillation was carried out was 45 ℃.
3. The method for passivating hydrazino nickel nitrate according to claim 1, wherein in the step (1), the coating agent is graphite and phenolic resin, the mass ratio of the phenolic resin to the graphite is 2:8, the solvent is alcohol, and 5-20wt% of graphite dispersion liquid is prepared; in step (3), the temperature at which the vacuum rotary distillation was carried out was 60 ℃.
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