CN114933819A - Method for preparing pigment carbon black from waste polydicyclopentadiene - Google Patents
Method for preparing pigment carbon black from waste polydicyclopentadiene Download PDFInfo
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- CN114933819A CN114933819A CN202210622758.3A CN202210622758A CN114933819A CN 114933819 A CN114933819 A CN 114933819A CN 202210622758 A CN202210622758 A CN 202210622758A CN 114933819 A CN114933819 A CN 114933819A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
- B01D39/083—Filter cloth, i.e. woven, knitted or interlaced material of organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/02—Particle separators, e.g. dust precipitators, having hollow filters made of flexible material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
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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
- C09C1/56—Treatment of carbon black ; Purification
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention relates to the technical field of recycling, and aims to solve the problems of poor heat resistance, easy blockage, poor filtering effect, low carbon black yield, repeated filtering and high cost of a filter bag used in the existing method for preparing pigment carbon black from waste polydicyclopentadiene, and in particular relates to a method for preparing pigment carbon black from waste polydicyclopentadiene; according to the method, nitrogen, carbon dioxide and air are mixed, oxygen required by combustion is provided, and simultaneously, non-combustible nitrogen and carbon dioxide are added, so that polydicyclopentadiene can be ignited but can not be combusted completely, a large amount of flocculent carbon black can be generated, then, the heat-resistant filter bag is used for filtering, the heat-resistant filter bag has a good filtering effect and high temperature resistance, and meanwhile, the filter bag has the advantage of being not easy to adhere, so that carbon black can be fully collected, the heat-resistant filter bag cannot be blocked, and the good filtering effect can be kept for a long time.
Description
Technical Field
The invention relates to the technical field of recycling, in particular to a method for preparing pigment carbon black from waste polydicyclopentadiene.
Background
The polydicyclopentadiene is a novel thermosetting engineering plastic, has excellent mechanical properties such as high impact strength, high modulus and the like, and good formability by a forming process, and is particularly suitable for being made into ultrathin parts with high strength and large area. Therefore, the material is widely applied to the fields of traffic vehicles, engineering machinery, chemical engineering environmental protection, national defense and military industry, medical treatment, sports equipment and the like. However, polydicyclopentadiene is difficult to recycle after being discarded, and has a serious adverse effect on the environment. With the widespread use of polydicyclopentadiene materials, the recycling of polydicyclopentadiene after disposal has attracted a great deal of attention.
At present, the waste polydicyclopentadiene products are mainly recycled by adopting a thermal cracking technology to be converted into combustible gas and liquid, and the residue is carbon black. However, the components are very complex and difficult to be used as common fuels, so that the fuel can be a potential secondary pollution source; residual carbon black can only be used as a low end scenario due to poor quality. The method has important significance for the research of eliminating the adverse effect of the waste polydicyclopentadiene on the environment and converting the waste polydicyclopentadiene into a product with higher added value.
Polydicyclopentadiene is a polymer with a high carbon content, and a large amount of flocculent carbon black is generated due to incomplete combustion when ignited, so that polydicyclopentadiene can be converted into high-quality pigment carbon black according to the characteristic. Compared with common carbon black, the pigment carbon black has the characteristics of small particle size and high blackness, and has higher value when being used as a coloring pigment in products such as printing ink, paint, coating, plastics and the like. The production process of pigment carbon black mainly adopts an oil furnace method and a tank method, wherein the former raw material is high aromatic hydrocarbon oil such as ethylene tar and anthracene oil, and the latter raw material is natural gas, coke oven gas or heavy liquid hydrocarbon, and the production process is complex, equipment is huge and complex and the cost is high. If the waste polydicyclopentadiene is used as the raw material, the preparation of the high-grade carbon black pigment by adopting the incomplete combustion process is technically feasible, and has great cost advantage.
However, the carbon black gas flow is required to be filtered by the filter bag to produce the pigment carbon black by utilizing incomplete combustion of polydicyclopentadiene, the carbon black gas flow carries a large amount of heat, the existing filter bag has poor heat resistance, is easy to be damaged and deformed by the heat carried by the carbon black gas flow, and causes poor filtering effect, low carbon black yield and easy blockage, if the pore diameter of the filter screen is required to be increased for blockage prevention, the filtering effect is poor, multiple times of filtering are required, and the cost is high.
How to improve the problems that the filter bag used in the existing method for preparing the pigment carbon black by using the waste polydicyclopentadiene has poor heat resistance, is easy to block, causes poor filtering effect and low carbon black yield, needs to be filtered for many times and has high cost is the key of the invention, and therefore, a method for preparing the pigment carbon black by using the waste polydicyclopentadiene is urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a method for preparing pigment carbon black from waste polydicyclopentadiene, which comprises the following steps: the method comprises the steps of mixing nitrogen, carbon dioxide and air to obtain mixed gas, introducing the mixed gas into a combustion chamber, putting waste polydicyclopentadiene into the combustion chamber containing the mixed gas, igniting the mixed gas, burning the mixed gas under an anoxic state to generate flocculent carbon black, introducing airflow containing the flocculent carbon black into a channel provided with a temperature-resistant filter bag, and collecting the airflow to obtain the pigment carbon black.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing pigment carbon black from waste polydicyclopentadiene comprises the following steps:
the method comprises the following steps: mixing nitrogen, carbon dioxide and air to obtain mixed gas, and introducing the mixed gas into a combustion chamber;
step two: putting the waste polydicyclopentadiene into a combustion chamber containing mixed gas, igniting the waste polydicyclopentadiene, and combusting the waste polydicyclopentadiene in an anoxic state to generate flocculent carbon black;
step three: the gas flow containing the flocculent carbon black is introduced into a channel provided with a temperature-resistant filter bag and is collected to obtain pigment carbon black, the generated combustion waste gas contains a small amount of carbon dioxide and methane, the combustion waste gas is introduced into a secondary combustion chamber to mix air for secondary combustion, and the tail gas is introduced into an activated carbon adsorption device to be adsorbed and then is discharged into the atmosphere.
As a further scheme of the invention: the temperature-resistant filter bag is prepared by the following steps:
s1: placing a self-made dianhydride monomer and a self-made diamine monomer in a vacuum drying oven, drying for 5-6h at the temperature of 80-85 ℃, then adding the self-made dianhydride monomer and N, N-dimethylacetamide into a three-neck flask provided with a stirrer and a thermometer, stirring for 20-30min at the temperature of 25-30 ℃ and the stirring speed of 500r/min, then adding the self-made diamine monomer into the three-neck flask by 3-5 times, wherein the adding amount of each time is the same, continuing stirring and reacting for 5-6h after the addition is finished, and then cooling to 5-10 ℃ to obtain a temperature-resistant spinning solution;
the reaction process is as follows:
s2: performing electrostatic spinning on the spinning solution to form a temperature-resistant fiber membrane, placing the temperature-resistant fiber membrane in a vacuum drying oven, drying for 3-4h at the temperature of 80-85 ℃, then placing the temperature-resistant fiber membrane in a muffle furnace, performing heat preservation and heat treatment for 30-40min at the temperature of 100 ℃, 200 ℃, 300 ℃ and 350 ℃ in sequence, and dehydrating amino and carboxyl in the molecule of the temperature-resistant fiber membrane to perform ring closure in the molecule to obtain a temperature-resistant filtering material;
the reaction process is as follows:
s3: and cutting and sewing the temperature-resistant filter material to obtain the temperature-resistant filter bag.
As a further scheme of the invention: the dosage ratio of the self-made dianhydride monomer, the self-made diamine monomer and the N, N-dimethylacetamide is 0.11 mol: 0.1 mol: 200-250 mL; the flow ratio of the nitrogen to the carbon dioxide to the air is 1-2.5: 1-2.5: 5-8.
As a further scheme of the invention: the preparation method of the self-made dianhydride monomer comprises the following steps:
a1: adding 1,2, 3-trichlorobenzene, sulfolane, potassium fluoride and tetrabutylammonium bromide into a three-neck flask provided with a stirrer, a thermometer and a gas-guide tube, introducing nitrogen for protection, stirring and reacting for 3-5h under the conditions that the temperature is 170-;
the reaction process is as follows:
a2: adding the intermediate 1 and dichloroethane into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, stirring for 20-30min at the temperature of 5-10 ℃ and at the stirring speed of 300-400r/min, then adding sodium bromide, sodium dihydrogen phosphate and deionized water, then dropwise adding a sodium hypochlorite solution while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 3-5h at the temperature of 10-13 ℃ after dropwise adding is finished, standing and layering a reaction product after the reaction is finished, washing an organic phase with distilled water for 2-3 times, drying with anhydrous magnesium sulfate, and then removing the solvent by rotary evaporation to obtain an intermediate 2;
the reaction process is as follows:
a3: adding the intermediate 2, anhydrous tetrahydrofuran and magnesium chips into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring and reacting for 2-3h under the conditions that the temperature is 70-75 ℃ and the stirring speed is 400r/min, then cooling to 5-10 ℃ while stirring and adding 1, 3, 5, 7-tetramethylcyclotetrasiloxane one by one, controlling the dropping speed to be 1-2 drops/s, continuing stirring and reacting for 1-2h after the dropping is finished, then dropwise adding a hydrochloric acid solution while stirring, controlling the dropping speed to be 1-2 drops/s, continuing stirring and reacting for 1-2h after the dropping is finished, standing and layering the reaction product after the reaction is finished, and rotationally evaporating an organic phase to remove the solvent to obtain an intermediate 3;
the reaction process is as follows:
a4: adding maleic anhydride, methanol and p-toluenesulfonic acid into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and heating to reflux at the stirring speed of 200-300r/min, stirring for reaction for 10-15h, and distilling the reaction product after the reaction is finished to remove unreacted methanol to obtain an intermediate 4;
the reaction process is as follows:
a5: adding the intermediate 4, anhydrous toluene and chloroplatinic acid solution into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a constant-pressure dropping funnel, introducing nitrogen for protection, stirring for 5-10min under the conditions that the temperature is 85-90 ℃ and the stirring speed is 400r/min, then dropwise adding the intermediate 3 solution while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 10-15h after the dropwise adding is finished, cooling the reaction product to room temperature after the reaction is finished to obtain an intermediate 5 solution, then adding dichloromethane, anhydrous methanol and sodium hydroxide into the intermediate 5 solution, stirring and reacting for 20-30h under the condition that the temperature is 25-30 ℃, adding the reaction product into distilled water for standing and layering after the reaction is finished, cooling the water phase to 0 ℃, then adjusting the pH to 0.5-1 by using concentrated hydrochloric acid, standing for 20-30h, carrying out vacuum filtration, washing the filter cake with distilled water for 2-3 times, then placing the filter cake in a vacuum drying oven, and drying for 10-15h at the temperature of 50-60 ℃ to obtain an intermediate 6;
the reaction process is as follows:
a6: adding the intermediate 6, acetic anhydride and xylene into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser tube, stirring and reacting for 20-30h at the temperature of 110-115 ℃ and the stirring rate of 300-350r/min, adding activated carbon after the reaction is finished, stirring for 2-3h at the temperature of 60-70 ℃, then performing vacuum filtration, adding the filtrate into anhydrous ether to precipitate out a precipitate, performing vacuum filtration, washing the filter cake for 2-3 times by using petroleum ether, then placing the filter cake into a vacuum drying box, and drying for 10-15h at the temperature of 120-130 ℃ to obtain the self-made dianhydride monomer.
The reaction process is as follows:
as a further scheme of the invention: the dosage ratio of the 1,2, 3-trichlorobenzene, the sulfolane, the potassium fluoride and the tetrabutylammonium bromide in the step A1 is 0.1 mol: 20-30 mL: 0.35-0.4 mol: 0.2-0.3 g.
As a further scheme of the invention: the dosage ratio of the intermediate 1, dichloroethane, sodium bromide, sodium dihydrogen phosphate, deionized water and sodium hypochlorite solution in the step A2 is 0.1 mol: 25-30 mL: 0.1 mol: 0.1 mol: 30-40 mL: 90-100g, wherein the mass fraction of the sodium hypochlorite solution is 10%.
As a further scheme of the invention: the dosage ratio of the intermediate 2, anhydrous tetrahydrofuran, magnesium chips, 1, 3, 5, 7-tetramethylcyclotetrasiloxane and hydrochloric acid solution in the step A3 is 0.1 mol: 30-40 mL: 0.11-0.13 mol: 0.25-0.3 mol: 18-22mL, wherein the mass fraction of the hydrochloric acid solution is 20-25%.
As a further scheme of the invention: the dosage ratio of the maleic anhydride, the methanol and the p-toluenesulfonic acid in the step A4 is 0.1 mol: 20-25 mL: 0.8-1.2 g.
As a further scheme of the invention: the dosage ratio of the intermediate 4, the anhydrous toluene, the chloroplatinic acid solution, the intermediate 3 solution, the dichloromethane, the anhydrous methanol and the sodium hydroxide in the step A5 is 0.02 mol: 15-20 mL: 2-3 mL: 10-15 mL: 150-200 mL: 25-30 mL: 2.5-4.0g, wherein the chloroplatinic acid solution is chloroplatinic acid according to the weight ratio of 1 g: 50mL of solution formed by dissolving the intermediate 3 in absolute ethyl alcohol, wherein the intermediate 3 solution is prepared by dissolving the intermediate 3 in 0.01mL of solution: 10mL of the solution is dissolved in anhydrous basically to form a solution, and the mass fraction of the concentrated hydrochloric acid is 35-38%.
As a further scheme of the invention: the using ratio of the intermediate 6, acetic anhydride, xylene and activated carbon in the step A6 is 0.1 mol: 60-80 mL: 30-40 mL: 3-5 g.
As a further scheme of the invention: the preparation method of the self-made diamine monomer comprises the following steps:
b1: adding hydroquinone and N, N-dimethylacetamide into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring for 10-15min under the conditions that the temperature is 120-, to obtain an intermediate 7;
the reaction process is as follows:
b2: adding reduced iron powder, ethanol solution and concentrated hydrochloric acid into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring at the temperature of 75-80 ℃ and the stirring rate of 300-400r/min for 25-30min, then cooling to 55-65 ℃, adding an intermediate 7, stirring while heating to 80-85 ℃, controlling the heating rate to be 2-3 ℃/min, then continuing to stir for 7-9h, after the reaction is finished, carrying out vacuum filtration on the reaction product, adjusting the pH of the filtrate to 8-8.5 by using sodium hydroxide solution, standing for 8-10h, then carrying out vacuum filtration, adding the filtrate into distilled water to precipitate, carrying out vacuum filtration, placing the filter cake into a vacuum drying box, drying at the temperature of 60-70 ℃ for 5-7h, to obtain the self-made diamine monomer.
The reaction process is as follows:
as a further scheme of the invention: the dosage ratio of the hydroquinone, the N, N-dimethylacetamide, the anhydrous potassium carbonate and the 2-chloro-5-nitrobenzotrifluoride solution in the step B1 is 0.1 mol: 80-100 mL: 0.11-0.12 mol: 0.22-0.24mol, wherein the ethanol solution is absolute ethanol and deionized water according to the volume ratio of 1: 1.
As a further scheme of the invention: the dosage ratio of the reduced iron powder, the ethanol solution, the concentrated hydrochloric acid and the intermediate 7 in the step B2 is 0.4-0.5 mol: 100-120 mL: 4-6 mL: 0.2mol, 80% of ethanol solution, 36-38% of concentrated hydrochloric acid and 1-2mol/L of sodium hydroxide solution.
The invention has the beneficial effects that:
the invention relates to a method for preparing pigment carbon black from waste polydicyclopentadiene, which comprises the steps of mixing nitrogen, carbon dioxide and air to obtain mixed gas, introducing the mixed gas into a combustion chamber, putting the waste polydicyclopentadiene into the combustion chamber containing the mixed gas, igniting the waste polydicyclopentadiene, combusting the waste polydicyclopentadiene in an anoxic state to generate flocculent carbon black, introducing airflow containing the flocculent carbon black into a channel provided with a temperature-resistant filter bag, and collecting the airflow to obtain the pigment carbon black; according to the method, nitrogen, carbon dioxide and air are mixed, oxygen required by combustion is provided, and simultaneously, non-combustible nitrogen and carbon dioxide are added, so that polydicyclopentadiene can be ignited but can not be combusted completely, a large amount of flocculent carbon black can be generated, then, the polydicyclopentadiene is filtered by using the temperature-resistant filter bag, the temperature-resistant filter bag has a good filtering effect and high temperature resistance, and meanwhile, the polydicyclopentadiene has the advantage of being not easy to adhere, so that carbon black can be fully collected, the temperature-resistant filter bag cannot be blocked, and the good filtering effect can be maintained for a long time;
the preparation method comprises the steps of firstly fluorinating 1,2, 3-trichlorobenzene by using potassium fluoride, introducing a large amount of F atoms to obtain an intermediate 1, then brominating the intermediate 1 by using sodium bromide to introduce bromine atoms to obtain an intermediate 2, then carrying out Grignard reaction on the intermediate 2 to introduce Si-O-Si bonds and Si-H bonds to obtain an intermediate 3, endowing the intermediate 3 with certain flexibility and low surface energy by the former, carrying out hydrosilylation reaction on the latter and a product intermediate 4 of maleic anhydride and methanol to generate an intermediate 5, hydrolyzing ester groups to form carboxyl groups to obtain an intermediate 6, dehydrating the intermediate 6 to form anhydride to obtain a self-made dianhydride monomer, then carrying out nucleophilic substitution reaction on hydroxyl on hydroquinone and chlorine atoms on 2-chloro-5-nitrobenzotrifluoride, introducing two nitro groups to obtain an intermediate 7, reducing the nitro groups on the intermediate 7 into amino groups by using reduced iron powder to obtain a self-made diamine monomer, dehydrating by using the self-made dianhydride monomer and the self-made diamine monomer to form an amide polymer to form a spinning solution, spinning the spinning solution to form a fiber membrane, and performing heat treatment on the fiber membrane to dehydrate the amino groups and carboxyl groups in the molecules of the amide polymer to form a closed loop in the molecules to obtain a temperature-resistant filter material; the molecular chain of the temperature-resistant filter material contains a large number of ring structures including benzene rings and nitrogen-containing heterocycles, the stability of the ring structures is high, the temperature-resistant filter material is endowed with certain high temperature resistance, molecules of the temperature-resistant filter material contain a large number of Si-O-Si bonds and C-F bonds, the bond energy is large, the polarities of the Si-O-Si bonds and the C-F bonds are large, a connected hydrocarbyl group can play a role in protection and shielding, the high temperature resistance of the temperature-resistant filter material is further improved, fluorine atoms have strong binding capacity for extra-nuclear electrons and bonding electron clouds, the polarizability of the C-F bonds is low, the acting force between polymer molecules containing the carbon-fluorine bonds is small, so that the fluorine-containing polymer has small surface tension and strong hydrophobic and oil-repellent capacity, and the temperature-resistant filter material is endowed with good anti-adhesion performance, thereby ensuring that the carbon black is not easy to adhere to the temperature-resistant filter material and block the temperature-resistant filter material; therefore, the high-temperature resistant filter material has good high-temperature resistance and anti-blocking effect under the synergistic action of a large number of ring structures, Si-O-Si bonds and C-F bonds.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the embodiment is a preparation method of a self-made dianhydride monomer, which comprises the following steps:
a1: adding 0.1mol of 1,2, 3-trichlorobenzene, 20mL of sulfolane, 0.35mol of potassium fluoride and 0.2g of tetrabutylammonium bromide into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, stirring and reacting for 3 hours under the conditions that the temperature is 170 ℃, the pressure is 2MPa and the stirring speed is 300r/min, distilling a reaction product after the reaction is finished to remove the sulfolane, and then cooling to room temperature to obtain an intermediate 1;
a2: adding 0.1mol of the intermediate 1 and 25mL of dichloroethane into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20min under the conditions that the temperature is 5 ℃ and the stirring speed is 300r/min, then adding 0.1mol of sodium bromide, 0.1mol of sodium dihydrogen phosphate and 30mL of deionized water, then dropwise adding 90g of a sodium hypochlorite solution with the mass fraction of 10% while stirring, controlling the dropping speed to be 1 drop/s, continuously stirring and reacting for 3h under the condition that the temperature is 10 ℃ after the dropping is finished, standing and layering reaction products after the reaction is finished, washing an organic phase with distilled water for 2 times, drying with anhydrous magnesium sulfate, and then removing the solvent by rotary evaporation to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 30mL of anhydrous tetrahydrofuran and 0.11mol of magnesium chips into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring and reacting for 2h under the conditions that the temperature is 70 ℃ and the stirring speed is 300r/min, then cooling to 5 ℃ while stirring and dropwise adding 0.25mol of 1, 3, 5, 7-tetramethylcyclotetrasiloxane, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 1h after the dropwise adding is finished, then dropwise adding 18mL of hydrochloric acid solution with the mass fraction of 20% while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 1h after the dropwise adding is finished, standing and layering a reaction product after the reaction is finished, and rotationally evaporating an organic phase to remove a solvent to obtain an intermediate 3;
a4: adding 0.1mol of maleic anhydride, 20mL of methanol and 0.8g of p-toluenesulfonic acid into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to reflux while stirring at a stirring speed of 200r/min, stirring for reaction for 10 hours, and distilling a reaction product after the reaction is finished to remove unreacted methanol to obtain an intermediate 4;
a5: 0.02mol of intermediate 4, 15mL of anhydrous toluene, 2mL of chloroplatinic acid were mixed in a ratio of 1 g: 50mL of chloroplatinic acid solution dissolved in absolute ethanol is added into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a constant-pressure dropping funnel, nitrogen is introduced for protection, the mixture is stirred for 5min under the conditions that the temperature is 85 ℃ and the stirring speed is 300r/min, and then 10mL of intermediate 3 is added dropwise under stirring according to the proportion of 0.01 mL: dissolving 10mL of intermediate 3 solution formed basically by anhydrous reaction, controlling the dropping rate to be 1 drop/s, continuing stirring and reacting for 10 hours after the dropping is finished, cooling a reaction product to room temperature after the reaction is finished to obtain an intermediate 5 solution, then adding 150mL of dichloromethane, 25mL of anhydrous methanol and 2.5g of sodium hydroxide into the intermediate 5 solution, stirring and reacting for 20 hours at the temperature of 25 ℃, adding the reaction product into distilled water for standing and layering after the reaction is finished, cooling a water phase to 0 ℃, then adjusting the pH to 0.5 by using concentrated hydrochloric acid with the mass fraction of 35%, then standing for 20 hours, carrying out vacuum filtration, washing a filter cake for 2 times by using distilled water, then placing in a vacuum drying oven, and drying for 10 hours at the temperature of 50 ℃ to obtain an intermediate 6;
a6: adding 0.1mol of intermediate 6, 60mL of acetic anhydride and 30mL of dimethylbenzene into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 20h at the temperature of 110 ℃ and the stirring rate of 300r/min, adding 3g of activated carbon after the reaction is finished, stirring for 2h at the temperature of 60 ℃, then carrying out vacuum filtration, adding filtrate into anhydrous ether to precipitate out a precipitate, carrying out vacuum filtration, washing a filter cake for 2 times by using petroleum ether, then placing the filter cake into a vacuum drying oven, and drying for 10h at the temperature of 120 ℃ to obtain the self-made dianhydride monomer.
Example 2:
the embodiment is a preparation method of a self-made dianhydride monomer, which comprises the following steps:
a1: adding 0.1mol of 1,2, 3-trichlorobenzene, 30mL of sulfolane, 0.4mol of potassium fluoride and 0.3g of tetrabutylammonium bromide into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, stirring and reacting for 5 hours under the conditions that the temperature is 175 ℃, the pressure is 2.2MPa and the stirring speed is 400r/min, distilling a reaction product after the reaction is finished to remove the sulfolane, and then cooling to room temperature to obtain an intermediate 1;
a2: adding 0.1mol of the intermediate 1 and 30mL of dichloroethane into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 30min under the conditions that the temperature is 10 ℃ and the stirring speed is 400r/min, then adding 0.1mol of sodium bromide, 0.1mol of sodium dihydrogen phosphate and 40mL of deionized water, then dropwise adding 100g of a sodium hypochlorite solution with the mass fraction of 10% while stirring, controlling the dropping speed to be 2 drops/s, continuously stirring and reacting for 5h under the condition that the temperature is 13 ℃ after the dropping is finished, standing and layering reaction products after the reaction is finished, washing an organic phase with distilled water for 3 times, drying with anhydrous magnesium sulfate, and then removing the solvent by rotary evaporation to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 40mL of anhydrous tetrahydrofuran and 0.13mol of magnesium chips into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring and reacting for 3h under the conditions that the temperature is 75 ℃ and the stirring speed is 400r/min, then cooling to 10 ℃ while stirring, dropwise adding 0.3mol of 1, 3, 5, 7-tetramethylcyclotetrasiloxane, controlling the dropwise adding speed to be 2 drops/s, continuously stirring and reacting for 2h after the dropwise adding is finished, then dropwise adding 22mL of hydrochloric acid solution with the mass fraction of 25% while stirring, controlling the dropwise adding speed to be 2 drops/s, continuously stirring and reacting for 2h after the dropwise adding is finished, standing and layering a reaction product after the reaction is finished, and rotationally evaporating an organic phase to remove a solvent to obtain an intermediate 3;
a4: adding 0.1mol of maleic anhydride, 25mL of methanol and 1.2g of p-toluenesulfonic acid into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to reflux while stirring at a stirring speed of 300r/min, stirring for reaction for 15 hours, and distilling a reaction product after the reaction is finished to remove unreacted methanol to obtain an intermediate 4;
a5: 0.02mol of intermediate 4, 20mL of anhydrous toluene, 3mL of chloroplatinic acid were added in an amount of 1 g: adding 50mL of chloroplatinic acid solution dissolved in absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant-pressure dropping funnel, introducing nitrogen for protection, stirring for 10min under the conditions that the temperature is 90 ℃ and the stirring speed is 400r/min, and then dropwise adding 15mL of intermediate 3 while stirring according to the proportion of 0.01 mL: dissolving 10mL of intermediate 3 solution formed basically by anhydrous reaction, controlling the dropping rate to be 2 drops/s, continuing stirring and reacting for 15 hours after the dropping is finished, cooling a reaction product to room temperature after the reaction is finished to obtain an intermediate 5 solution, then adding 200mL of dichloromethane, 30mL of anhydrous methanol and 4.0g of sodium hydroxide into the intermediate 5 solution, stirring and reacting for 30 hours at the temperature of 30 ℃, adding the reaction product into distilled water for standing and layering after the reaction is finished, cooling a water phase to 0 ℃, then adjusting the pH to 1 by using concentrated hydrochloric acid with the mass fraction of 38%, then standing for 30 hours, carrying out vacuum filtration, washing a filter cake for 3 times by using the distilled water, then placing the filter cake in a vacuum drying box, and drying for 15 hours at the temperature of 60 ℃ to obtain an intermediate 6;
a6: adding 0.1mol of intermediate 6, 80mL of acetic anhydride and 40mL of xylene into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 30h at the temperature of 115 ℃ and the stirring rate of 350r/min, adding 5g of activated carbon after the reaction is finished, stirring for 3h at the temperature of 0 ℃, then carrying out vacuum filtration, adding the filtrate into anhydrous ether to separate out a precipitate, carrying out vacuum filtration, washing a filter cake for 3 times by using petroleum ether, then placing the filter cake into a vacuum drying oven, and drying for 15h at the temperature of 130 ℃ to obtain the self-made dianhydride monomer.
Example 3:
this example is a method for preparing a self-made diamine monomer, comprising the following steps:
b1: adding 0.1mol of hydroquinone, 80mLN, N-dimethylacetamide into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring for 10min under the conditions that the temperature is 120 ℃ and the stirring rate is 350r/min, then adding 0.11mol of anhydrous potassium carbonate, continuously stirring for 10min, then dropwise adding 0.22mol of 2-chloro-5-nitrotrifluorotoluene solution while stirring, controlling the dropwise adding rate to be 1 drop/s, heating to 150 ℃ after the dropwise adding is finished, continuously stirring for reaction for 20h, cooling a reaction product to room temperature after the reaction is finished, carrying out vacuum filtration, and adding a filtrate to a mixture of anhydrous ethanol and deionized water according to the volume ratio of 1: 1, precipitating out a precipitate in an ethanol solution formed by mixing, carrying out vacuum filtration, placing a filter cake in a vacuum drying oven, and drying for 8 hours at the temperature of 60 ℃ to obtain an intermediate 7;
b2: 0.4mol of reduced iron powder, 100mL of an 80% ethanol solution by volume fraction, and 4mL of concentrated hydrochloric acid of 36% by mass fraction were charged into a three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, stirring for 25min under the conditions that the temperature is 75 ℃ and the stirring speed is 300r/min, then cooling to 55 ℃, adding 0.2mol of the intermediate 7, heating to 80 ℃ while stirring, controlling the heating speed to be 2 ℃/min, then continuously stirring for reaction for 7h, after the reaction is finished, carrying out vacuum filtration on a reaction product, adjusting the pH of a filtrate to 8 by using a sodium hydroxide solution with the molar concentration of 1mol/L, standing for 8h, then carrying out vacuum filtration, adding the filtrate into distilled water to precipitate, carrying out vacuum filtration, placing a filter cake into a vacuum drying oven, and drying for 5h under the condition that the temperature is 60 ℃ to obtain the self-made diamine monomer.
Example 4:
this example is a method for preparing a self-made diamine monomer, comprising the following steps:
b1: adding 0.1mol of hydroquinone and 100mLN, N-dimethylacetamide into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser and a constant-pressure dropping funnel, stirring for 15min under the conditions that the temperature is 130 ℃ and the stirring rate is 450r/min, then adding 0.12mol of anhydrous potassium carbonate, continuously stirring for 15min, then dropwise adding 0.24mol of 2-chloro-5-nitrobenzotrifluoride solution while stirring, controlling the dropwise adding rate to be 2 drops/s, heating to 155 ℃ after the dropwise adding is finished, continuously stirring for reaction for 30h, cooling a reaction product to room temperature after the reaction is finished, carrying out vacuum filtration, and adding a filtrate to a state that the volume ratio of absolute ethyl alcohol to deionized water is 1: 1, precipitating out a precipitate from an ethanol solution formed by mixing, carrying out vacuum filtration, placing a filter cake in a vacuum drying oven, and drying for 10 hours at the temperature of 70 ℃ to obtain an intermediate 7;
b2: 0.5mol of reduced iron powder, 120mL of an ethanol solution with a volume fraction of 80% and 6mL of concentrated hydrochloric acid with a mass fraction of 38% are added into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser tube, stirring for 30min under the conditions that the temperature is 80 ℃ and the stirring speed is 400r/min, then cooling to 65 ℃, adding 0.2mol of the intermediate 7, heating to 85 ℃ while stirring, controlling the heating speed to be 3 ℃/min, then continuing stirring for reaction for 9h, after the reaction is finished, carrying out vacuum filtration on a reaction product, adjusting the pH of a filtrate to be 8.5 by using a sodium hydroxide solution with the molar concentration of 2mol/L, standing for 10h, then carrying out vacuum filtration, adding the filtrate into distilled water to precipitate, carrying out vacuum filtration, placing a filter cake into a vacuum drying oven, and drying for 7h under the condition that the temperature is 70 ℃ to obtain the self-made diamine monomer.
Example 5:
in this embodiment, the temperature-resistant filter bag is prepared by the following steps:
s1: placing 0.11mol of the self-made dianhydride monomer from example 3 and 0.1mol of the self-made diamine monomer from example 5 in a vacuum drying oven, drying at 80 ℃ for 5h, adding the self-made dianhydride monomer and 250mLN, N-dimethylacetamide into a three-neck flask provided with a stirrer and a thermometer, stirring at 25 ℃ and at a stirring speed of 300r/min for 20min, adding the self-made diamine monomer into the three-neck flask for 3 times, wherein the adding amount is the same for each time, continuously stirring for reacting for 5h after the addition is finished, and cooling to 5 ℃ to obtain a temperature-resistant spinning solution;
s2: performing electrostatic spinning on the spinning solution to form a temperature-resistant fiber membrane, placing the temperature-resistant fiber membrane in a vacuum drying oven, drying for 3h at the temperature of 80 ℃, then placing the fiber membrane in a muffle furnace, performing heat preservation and heat treatment for 30min at the temperatures of 100 ℃, 200 ℃, 300 ℃ and 350 ℃ in sequence, dehydrating amino and carboxyl in the molecules of the temperature-resistant fiber membrane, and performing ring closure in the molecules to obtain a temperature-resistant filter material;
s3: and cutting and sewing the temperature-resistant filter material to obtain the temperature-resistant filter bag.
Example 6:
in this embodiment, the temperature-resistant filter bag is prepared by the following steps:
s1: placing 0.11mol of the self-made dianhydride monomer from example 2 and 0.1mol of the self-made diamine monomer from example 4 in a vacuum drying oven, drying at 85 ℃ for 6h, adding the self-made dianhydride monomer and 200mLN, N-dimethylacetamide into a three-neck flask provided with a stirrer and a thermometer, stirring at the temperature of 30 ℃ and the stirring rate of 500r/min for 30min, adding the self-made diamine monomer into the three-neck flask for 5 times, wherein the adding amount of each time is the same, continuously stirring and reacting for 6h after the addition is finished, and cooling to 10 ℃ to obtain a temperature-resistant spinning solution;
s2: performing electrostatic spinning on the spinning solution to form a temperature-resistant fiber membrane, placing the temperature-resistant fiber membrane in a vacuum drying oven, drying for 4 hours at the temperature of 85 ℃, then placing the fiber membrane in a muffle furnace, performing heat preservation and heat treatment for 40 minutes at the temperature of 100 ℃, 200 ℃, 300 ℃ and 350 ℃ in sequence, dehydrating amino and carboxyl in the molecules of the temperature-resistant fiber membrane, and performing ring closure in the molecules to obtain a temperature-resistant filter material;
s3: and cutting and sewing the temperature-resistant filter material to obtain the temperature-resistant filter bag.
The performance of the temperature resistant filter bags of examples 5-6 were tested and the results are shown in the following table:
referring to the data in the table, it can be known that the temperature-resistant filter bag in the invention has high filtering efficiency and low filtering resistance, which means that the temperature-resistant filter bag has high filtering efficiency and good air permeability, thereby indicating that the filtering effect of the temperature-resistant filter bag is good, and the surface energy of the temperature-resistant filter bag is low, indicating that the anti-sticking property of the temperature-resistant filter bag is good, and the carbon black is not easy to stick, thereby having high yield and difficult to block, and meanwhile, the initial weight loss temperature of the temperature-resistant filter bag is high, and the weight loss at 300 ℃ and 600 ℃ is low, which indicates that the temperature-resistant filter bag has good high temperature resistance.
Example 7:
the embodiment is a method for preparing pigment carbon black from waste polydicyclopentadiene, which comprises the following steps:
the method comprises the following steps: nitrogen, carbon dioxide and air are mixed according to a flow ratio of 1.5: 1.5: 7, mixing to obtain mixed gas, and introducing the mixed gas into a combustion chamber;
step two: putting the waste polydicyclopentadiene into a combustion chamber containing mixed gas, igniting the waste polydicyclopentadiene, and combusting the waste polydicyclopentadiene in an anoxic state to generate flocculent carbon black;
step three: the gas flow containing flocculent carbon black is introduced into a channel provided with the temperature-resistant filter bag in the embodiment 6 and collected to obtain pigment carbon black, the generated combustion waste gas contains a small amount of carbon dioxide and methane, the combustion waste gas is introduced into a secondary combustion chamber to be mixed with air for secondary combustion, and the tail gas is introduced into an activated carbon adsorption device to be adsorbed and then is discharged into the atmosphere.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. A method for preparing pigment carbon black from waste polydicyclopentadiene is characterized by comprising the following steps:
the method comprises the following steps: mixing nitrogen, carbon dioxide and air to obtain mixed gas, and introducing the mixed gas into a combustion chamber;
step two: putting the waste polydicyclopentadiene into a combustion chamber containing mixed gas and igniting to generate flocculent carbon black;
step three: introducing the gas flow containing the flocculent carbon black into a channel provided with a temperature-resistant filter bag, and collecting the gas flow to obtain pigment carbon black;
the temperature-resistant filter bag is prepared by the following steps:
s1: drying a self-made dianhydride monomer and a self-made diamine monomer, adding the self-made dianhydride monomer and N, N-dimethylacetamide into a three-neck flask, stirring, adding the self-made diamine monomer into the three-neck flask for several times, wherein the adding amount of the self-made diamine monomer is the same for each time, continuing stirring and reacting after the addition is finished, and then cooling to obtain a temperature-resistant spinning solution;
s2: performing electrostatic spinning on the spinning solution to form a temperature-resistant fiber membrane, drying the temperature-resistant fiber membrane in a vacuum drying oven, and then performing heat preservation and heat treatment in a muffle furnace to obtain a temperature-resistant filtering material;
s3: and cutting and sewing the temperature-resistant filter material to obtain the temperature-resistant filter bag.
2. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 1, wherein the self-made dianhydride monomer, the self-made diamine monomer and the N, N-dimethylacetamide are used in an amount ratio of 0.11 mol: 0.1 mol: 200-250 mL; the flow ratio of the nitrogen to the carbon dioxide to the air is 1-2.5: 1-2.5: 5-8.
3. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 1, wherein the method for preparing self-made dianhydride monomer comprises the following steps:
a1: adding 1,2, 3-trichlorobenzene, sulfolane, potassium fluoride and tetrabutylammonium bromide into a three-neck flask, stirring for reaction, distilling a reaction product after the reaction is finished, and cooling to room temperature to obtain an intermediate 1;
a2: adding the intermediate 1 and dichloroethane into a three-neck flask, stirring, adding sodium bromide, sodium dihydrogen phosphate and deionized water, dropwise adding a sodium hypochlorite solution while stirring, continuing stirring for reaction after dropwise adding is finished, standing and layering a reaction product after the reaction is finished, and washing, drying and rotationally evaporating an organic phase to obtain an intermediate 2;
a3: adding the intermediate 2, anhydrous tetrahydrofuran and magnesium chips into a four-neck flask, stirring for reaction, cooling, adding 1, 3, 5, 7-tetramethylcyclotetrasiloxane dropwise while stirring, continuing to stir for reaction after the dropwise addition is finished, adding a hydrochloric acid solution dropwise while stirring, continuing to stir for reaction after the dropwise addition is finished, standing and layering reaction products after the reaction is finished, and rotationally evaporating an organic phase to obtain an intermediate 3;
a4: adding maleic anhydride, methanol and p-toluenesulfonic acid into a three-neck flask, heating to reflux while stirring, stirring for reaction, and distilling a reaction product after the reaction is finished to obtain an intermediate 4;
a5: adding the intermediate 4, anhydrous toluene and chloroplatinic acid solution into a three-neck flask, stirring, dropwise adding the intermediate 3 solution while stirring, continuously stirring for reaction after dropwise adding, cooling a reaction product to room temperature after the reaction is finished to obtain an intermediate 5 solution, then adding dichloromethane, anhydrous methanol and sodium hydroxide into the intermediate 5 solution for stirring reaction, adding the reaction product into distilled water after the reaction is finished, standing for layering, cooling a water phase, adjusting the pH value, standing, performing vacuum filtration, washing a filter cake, and drying to obtain an intermediate 6;
a6: adding the intermediate 6, acetic anhydride and xylene into a three-neck flask, stirring for reaction, adding activated carbon after the reaction is finished, continuously stirring, then carrying out vacuum filtration, adding the filtrate into anhydrous ether to precipitate, carrying out vacuum filtration, washing and drying the filter cake to obtain the self-made dianhydride monomer.
4. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 3, wherein the amount ratio of 1,2, 3-trichlorobenzene, sulfolane, potassium fluoride and tetrabutylammonium bromide in the step A1 is 0.1 mol: 20-30 mL: 0.35-0.4 mol: 0.2-0.3 g; the dosage ratio of the intermediate 1, dichloroethane, sodium bromide, sodium dihydrogen phosphate, deionized water and sodium hypochlorite solution in the step A2 is 0.1 mol: 25-30 mL: 0.1 mol: 0.1 mol: 30-40 mL: 90-100g, wherein the mass fraction of the sodium hypochlorite solution is 10%.
5. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 3, wherein the intermediate 2, anhydrous tetrahydrofuran, magnesium chips, 1, 3, 5, 7-tetramethylcyclotetrasiloxane and hydrochloric acid solution in the step A3 are used in an amount ratio of 0.1 mol: 30-40 mL: 0.11-0.13 mol: 0.25-0.3 mol: 18-22mL, wherein the mass fraction of the hydrochloric acid solution is 20-25%; the dosage ratio of the maleic anhydride, the methanol and the p-toluenesulfonic acid in the step A4 is 0.1 mol: 20-25 mL: 0.8-1.2 g.
6. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 3, wherein the amount ratio of the intermediate 4, the anhydrous toluene, the chloroplatinic acid solution, the intermediate 3 solution, the dichloromethane, the anhydrous methanol and the sodium hydroxide in step A5 is 0.02 mol: 15-20 mL: 2-3 mL: 10-15 mL: 150-200 mL: 25-30 mL: 2.5-4.0g, wherein the chloroplatinic acid solution is chloroplatinic acid according to the weight ratio of 1 g: 50mL of solution formed by dissolving the intermediate 3 in absolute ethyl alcohol, wherein the concentration of the intermediate 3 in the solution is 0.01 mL: 10mL of a solution formed by dissolving in anhydrous base; the using ratio of the intermediate 6, acetic anhydride, xylene and activated carbon in the step A6 is 0.1 mol: 60-80 mL: 30-40 mL: 3-5 g.
7. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 1, wherein the method for preparing the self-made diamine monomer comprises the following steps:
b1: adding hydroquinone and N, N-dimethylacetamide into a four-neck flask, stirring, adding anhydrous potassium carbonate, continuously stirring, dropwise adding a 2-chloro-5-nitrobenzotrifluoride solution while stirring, heating after dropwise adding, continuously stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, performing vacuum filtration, adding a filtrate into an ethanol solution to separate out a precipitate, performing vacuum filtration, and drying a filter cake to obtain an intermediate 7;
b2: adding reduced iron powder, an ethanol solution and concentrated hydrochloric acid into a three-neck flask, stirring, cooling, adding an intermediate 7, stirring while heating, continuing stirring for reaction, carrying out vacuum filtration on a reaction product after the reaction is finished, adjusting the pH of a filtrate, standing, carrying out vacuum filtration, adding the filtrate into distilled water, precipitating, carrying out vacuum filtration, and drying a filter cake to obtain the self-made diamine monomer.
8. The method for preparing pigment carbon black from waste polydicyclopentadiene according to claim 7, wherein the dosage ratio of hydroquinone, N-dimethylacetamide, anhydrous potassium carbonate and 2-chloro-5-nitrobenzotrifluoride solution in step B1 is 0.1 mol: 80-100 mL: 0.11-0.12 mol: 0.22-0.24mol, wherein the ethanol solution is absolute ethanol and deionized water according to the volume ratio of 1: 1; the dosage ratio of the reduced iron powder, the ethanol solution, the concentrated hydrochloric acid and the intermediate 7 in the step B2 is 0.4-0.5 mol: 100-120 mL: 4-6 mL: 0.2mol, 80% of ethanol solution in volume percentage, and 36-38% of concentrated hydrochloric acid in mass percentage.
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| CN117417542A (en) * | 2023-10-18 | 2024-01-19 | 湖北英采化学有限公司 | High-strength Wen Jiangnian early-strength-resistant dispersing agent |
| CN117417542B (en) * | 2023-10-18 | 2024-04-19 | 湖北英采化学有限公司 | High-resistant Wen Jiangnian early-strength dispersing agent |
| CN117417542B8 (en) * | 2023-10-18 | 2024-06-07 | 湖北英采化学有限公司 | High-resistant Wen Jiangnian early-strength dispersing agent |
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