CN115819240A - Nucleating agent and preparation method thereof and preparation method of polymer rod-shaped superfine powder - Google Patents
Nucleating agent and preparation method thereof and preparation method of polymer rod-shaped superfine powder Download PDFInfo
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Abstract
The invention discloses a nucleating agent, a preparation method thereof and a preparation method of polymer rod-shaped superfine powder. The structural formula of the nucleating agent is
Description
Technical Field
The invention belongs to the field of preparation of high molecular materials, and particularly relates to a form of a polymer, and more particularly relates to a preparation method of polymer powder.
Background
The special polymer superfine powder is a kind of basic raw material which can be used for material modification, paint preparation and other applications, and has special application. For example, the polyethersulfone ultrafine powder can be used for heat-resistant coatings, and for example, inner decorative coatings of civil aviation science and technology are all polyethersulfone materials; the non-stick pan coating may also be a polyethersulfone or polyetheretherketone coating, or the like. For some special polymers, because the structures of the polymers have rigid structures such as benzene rings and the like, the materials are not easy to break due to excellent mechanical properties, so that the preparation of ultrafine powder is difficult. In some special fields, it is necessary to modify them with special polymer materials.
Solution polymerization is a method for synthesizing macromolecules, and is a method for carrying out polymerization reaction on one or more monomers in a solution to produce a special polymer solution. Some polymer solutions are relatively easy to remove by devolatilization (e.g., polyoxymethylene, polyolefin elastomers, etc.) and pelletize to obtain polymer pellets. Some special polymerization needs to be synthesized in a strong polar solvent, and the strong polar solvent has the characteristics of high boiling point, high temperature, easiness in decomposition, difficulty in removal and the like, so that the removal is difficult by a devolatilization method. Therefore, the solution needs to be mixed with an inert solvent (miscible with a strong polar solvent, and immiscible with a polymer) to cause phase change precipitation of the polymer in the solution, so as to obtain the polymer. The precipitated polymer is in a block shape, so that the polymer needs to be crushed into small blocks, sheets, particles or powder by using crushing equipment, the crushed substance is washed by using a corresponding inert solvent, residual solvent or other impurities are washed, and the final product is obtained by drying, granulating and other steps. The polymer produced by this method is, for example, soluble polyimide (Ultem, aurumn), sulfone polymer (PSU, PPSU, PES), ketone Polymer (PEEK), polyphenylene sulfide (PPS) aromatic polyamide pulp (1313 or 1414), organic cellulose (cellulose acetate butyrate), PVDF, or the like.
At present, besides the precipitation fragmentation method, there are other methods to precipitate the polymer in the special polymer solution, such as adding stirring to the solution and adding an inert solvent while stirring, as described in patent CN102888003A, for example, the method of precipitation of sulfone polymer solution. However, the time required for the addition of the inert solution is slow, since the increase in the inert solvent causes the sulfone polymer to precipitate into a mass. Moreover, the salts in the course of the reaction are dissolved by water and cannot be separated. The patent CN105330840A describes a method of crushing after cooling by a cooling belt, but does not mention a specific method.
The special polymers such as imide polymer, sulfone polymer, polyphenylene sulfide, polyether ether ketone and the like have strong toughness, and continuous circulating crushing is needed in crushing equipment to crush to the expected effect. Otherwise, if the crushed particle size is too large, some impurities can be wrapped in the crushed particle size and cannot be removed, and the product quality can be influenced after drying and granulation. However, the solution of the material can be separated out into strips immediately after contacting with the mutually soluble inert solvent, and the solution blocks pipelines and equipment. Therefore, how to feed the materials to be smoothly separated out and quickly crushed without blocking pipelines and equipment is the first step for solving the problem. However, if the particle size of the crushed material is too large, the expected particle size effect cannot be achieved.
For wet material grinding, the ground form also has an influence on the product performance. In general, bulk density of special polymers such as polysulfone and polyetherimide after pulverization is relatively small, but particles are large and state is not uniform. In addition, usually, the powder of the special polymer is spherical after being pulverized. When the spherical powder is used for modifying other materials, uneven mixing is often caused by the deviation of the bulk density of the spherical powder, and particularly when glass fibers and carbon fibers are added for modification, unsmooth marks on the surface can be obviously seen after the special polymer powder added with the glass fibers and the carbon fibers is granulated. If the special polymer is crushed into a rod-shaped structure, the possibility of mutual hooking of the special polymer is increased, so that the glass fiber, the carbon fiber and the special polymer form good winding performance, and the uniformity of the mixed special polymer is facilitated. In a traditional method for separating a polymer from a polar solvent, the solution is usually precipitated or rolled into blocks by an inert solvent, solids are separated by solid-liquid separation, and the solid is crushed by a wet crusher, so that the efficiency is low. Therefore, the problem to be solved is how to solve the problem that the special polymer is not uniform in shape and size after being crushed and prepare powder in a rod shape.
Disclosure of Invention
The invention provides a nucleating agent, a preparation method thereof and a preparation method of polymer rod-shaped superfine powder. Due to the use of the nucleating agent, a rod-like form can be easily formed during pulverization, and the particle size is small, so that the bulk density of the powder is higher than that of powder obtained by precipitation pulverization in other ways.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
the invention provides a nucleating agent, which has the following structural formula:
wherein R 'or R' are independently benzene ring, biphenyl, acene or polybiphenyl, polyacene and derivatives thereof, preferably benzene ring; r represents an aliphatic hydrocarbon group of 2 to 4 carbons such as: -CH 2 -、-(CH 2 ) 2 -、-(CH 2 ) 3 -and the like; x or Y represents halogen, preferably Cl, br, X and Y may be the same or different.
The preparation method of the nucleating agent comprises the following steps: reacting halogenated aromatic anhydride with aliphatic hydrocarbon diol.
As a preferred scheme, the preparation method of the nucleating agent comprises the following steps: the halogenated aromatic anhydride and aliphatic hydrocarbon diol are refluxed in a hydrocarbon solvent to generate water, azeotropic dehydration is carried out, and after the solvent is evaporated, a solid is obtained and recrystallized.
In the preparation method of the nucleating agent, the molar ratio of the halogenated aromatic anhydride to the aliphatic hydrocarbon diol is 2.
The halogenated aromatic anhydride comprises but is not limited to one or more of 4-chlorophthalic anhydride, 3-bromophenylic anhydride and 4-bromophenylic anhydride.
The aliphatic hydrocarbon diol of the invention includes but is not limited to one or more of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol and 1, 4-butylene glycol.
The hydrocarbon solvent is one or more of aromatic hydrocarbon, aliphatic hydrocarbon or halogenated hydrocarbon with the boiling point of more than 170 ℃, and comprises but is not limited to n-decane, chloro-o-xylene (containing 3-chloro-o-xylene and/or 4-chloro-o-xylene), dichlorobenzene and the like.
In the preparation method of the nucleating agent, the reaction temperature is the reflux temperature of the solvent. The reaction time is 2 to 5 hours.
In the preparation method of the nucleating agent, the mass ratio of the halogenated aromatic anhydride to the aliphatic hydrocarbon diol to the hydrocarbon solvent is 1.
As a preferred embodiment, the recrystallization according to the present invention comprises the following steps: recrystallizing the solid with methanol or ethanol, wherein the mass ratio of the alcohol to the solid is 5-20; the recrystallization time is 1 to 5 hours, and the temperature is 60 to 75 ℃; and filtering and vacuum drying after recrystallization to obtain the nucleating agent.
A method for preparing polymer rod-like superfine powder comprises the following steps: mixing the polymer, nucleating agent and solvent, precipitating and crushing.
As a preferred scheme, the preparation method of the polymer rod-shaped ultrafine powder comprises the following steps: mixing polymer solution of polymer, nucleating agent and solvent with inert solvent, precipitating polymer, and pulverizing into slurry to obtain polymer rod-like superfine powder.
As a preferred scheme, the preparation method of the polymer rod-shaped ultrafine powder comprises the following steps: the settling tank with stirring, the polymer solution feeding pipe and the high-speed crushing equipment are connected to form a circulating crushing system. Adding an inert solvent into a precipitation tank, circulating the inert solvent in a system after a high-speed crushing device is started, adding a polymer solution of a polymer, a nucleating agent and a solvent into the inert solvent, precipitating the polymer into a solid strip after the polymer solution meets the inert solvent, and crushing the solid strip into slurry in the high-speed crushing device; after the feeding of the polymer solution is completed, the cyclic pulverization is maintained.
After the stacking density of the wet powder material is crushed to 0.35g/ml, a discharge valve and solid-liquid separation equipment are opened in the process of continuously crushing by high-speed crushing equipment, a part of slurry is extracted for solid-liquid separation to obtain polymer rod-shaped ultrafine powder, and the rest of slurry is continuously and circularly crushed.
In the preparation method of the polymer rod-shaped superfine powder, the ratio of the extraction amount to the circulation amount is 1.
The polymers described herein include, but are not limited to, imide polymers, sulfone polymers, ketone polymers, polyurethanes, aromatic polyamides, celluloses, fluoropolymers, and the like, preferably polyetherimides, polysulfones, polyphenylsulfones, polyethersulfones, polyphenylene sulfides, polyetheretherketones, and the like.
The solvent of the polymer solution comprises one or more of N, N-dimethylacetamide, N-methylpyrrolidone, sulfolane, dimethyl sulfoxide, N-dimethylformamide, acetic acid and butyric acid.
The mass ratio of the nucleating agent to the polymer is 1.
The dosage of the polymer solution and the inert solvent is based on the principle that the solid content of the crushed slurry in a solid-liquid mixing system can enable the solid-liquid mixed slurry to flow smoothly, and the mass ratio of the crushed slurry to the inert solvent is 1.
The inert solvent described in the present invention can only be miscible with the solvent in the polymer solution, but not dissolve the polymer, and includes but is not limited to one or more of water, ethanol, methanol, isopropanol, toluene, and xylene, preferably water.
The high-speed pulverizing apparatus of the present invention may be used in continuous wet pulverizing apparatuses including, but not limited to, a pulverizing pump, a colloid mill, a marine pulverizing pump, a grinder, etc.
The nucleating agent with the structure is added into the polymer solution, so that the secondary structure of the polymer during precipitation can be changed, and the crushed shape of the polymer is changed into a rod shape.
In the present invention, the kind and amount of the nucleating agent are main factors affecting the morphology of the polymer after pulverization.
The invention has the beneficial effects that:
(1) The method adopts the nucleating agent, so that the polymer is regularly precipitated, the continuous feeding and crushing can be realized, and the precipitation and crushing processes can be solved by using one crushing device.
(2) The nucleating agent is dissolved in a solvent to form a uniform solution with the polymer, so that the softness of precipitates can be increased, and a rod-shaped form can be easily formed during crushing.
(3) Due to the use of the nucleating agent, the polymer is in an aggregation state in the precipitation process, so that the bulk density of the polymer is higher than that of powder obtained by precipitation and crushing in other modes, the obtained material powder is convenient to wash and the volume of the powder is greatly reduced. The particle size of the powder is also far smaller than that obtained by crushing in other modes.
Drawings
FIG. 1 is a rod-shaped powder of example 1;
FIG. 2 shows a state after pulverization in comparative example 1;
FIG. 3 shows a pulverized state of comparative example 3;
FIG. 4 is a process flow diagram of example 1.
Detailed Description
Example 1
1. Preparation of nucleating agent:
A5L reactor was charged with 182.5g of 4-chlorophthalic anhydride, 31g of ethylene glycol, and 427g of n-decane, and the mixture was refluxed at 175 ℃ for 5 hours to remove water produced during the reflux. The vacuum was turned on, the vacuum was gradually pumped to near-0.1 MPa and the solvent was evaporated to dryness. Cooling to normal temperature, adding 888g of methanol into the reaction kettle, recrystallizing for 5 hours at 60 ℃, filtering and drying in vacuum to obtain the nucleating agent.
Table 1 shows the absorption wavenumbers of the characteristic groups of the infrared spectrum of the nucleating agent of example 1.
TABLE 1
2. And (3) a crushing process:
dissolving a nucleating agent and polysulfone particles with the diameter of 2-3 mm in a DMAC solution at a mass ratio of 1 3 H is used as the reference value. When the polysulfone solution is added, the average particle size of the pulverized powder is 10-50 μm, the bulk density of the wet material is 0.30g/ml, the feeding valve b is closed, and after the cyclic pulverization is continued for 30min, the bulk density is 0.35g/ml, the average particle size is 5-35 μm, and the product is rod-shaped. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
Example 2
1. Preparation of nucleating agent:
A5L reactor was charged with 182.5g of 4-chlorophthalic anhydride, 38g of 1, 2-propanediol, 662g of a mixture of 3-chloro-o-xylene and 4-chloro-o-xylene (mass ratio: 55), heated to 187 ℃ and refluxed for 2 hours, and water produced in the reaction was removed at the time of reflux. The vacuum was turned on, the vacuum was gradually pumped to near absolute pressure and the solvent was evaporated. Cooling to normal temperature, adding 1476g of methanol into the reaction kettle, recrystallizing at 65 ℃ for 4 hours, filtering and drying in vacuum to prepare the nucleating agent.
2. And (3) crushing:
the mass ratio of nucleating agent to polyamide-imide particles with the diameter of 2-3 mm is 2:1000 was dissolved in NMP to give a 26wt% polymer solution. Adding water into the precipitation tank, starting stirring, starting a crushing pump to circulate the water, adding a polymer solution for crushing, wherein the ratio of the feeding flow rate of the polymer solution to the water flow rate is 1 3 H is used as the reference value. When the polyamide-imide solution is completely added, the average grain diameter of the pulverized powder is 12-53 mu m, the bulk density of the wet material is 0.31g/ml, the feeding valve b is closed, the pulverized powder is continuously pulverized for 30min, the bulk density is 0.36g/ml, the average grain diameter is 5-35 mu m, and the product is rod-shaped. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
Example 3
1. Preparation of nucleating agent:
182.5g of 4-chlorophthalic anhydride, 38g of 1, 3-propanediol and 1103g of dichlorobenzene are added into a 5L reaction kettle, and the mixture is heated to 180 ℃ and refluxed for 4 hours, and water generated in the reaction is separated out during the reflux. The vacuum was turned on, the vacuum was gradually pumped to near absolute pressure and the solvent was evaporated. Cooling to normal temperature, adding 1845g of ethanol into the reaction kettle, recrystallizing for 3 hours at 70 ℃, filtering and drying in vacuum to prepare the nucleating agent.
2. And (3) crushing:
the nucleating agent and the diameter of 2 to 3mm polyphenylsulfone particles are mixed according to the mass ratio of 3:1000 was dissolved in sulfolane to make a 33wt% solution of polyphenylsulfone. Adding water into a precipitation tank, starting stirring, starting a crushing pump to circulate the water, adding a polymer solution for crushing, wherein the ratio of the feeding flow rate of the polyphenylsulfone solution to the water flow rate is 1 3 H is used as the reference value. When the polyphenylsulfone solution is completely added, the average grain diameter of the pulverized powder is 15-55 μm, the bulk density of the wet material is 0.33g/ml, the valve b is closed, the pulverized powder is continuously pulverized for 30min, the bulk density is 0.37g/ml, the average grain diameter is 5-35 μm, and the product is in a rod shape. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
Example 4
1. Preparation of nucleating agent:
A10L reaction vessel was charged with 227g of 4-bromobenzoic anhydride, 45g of 1, 4-butanediol, 2176g of a mixture of 3-chloro-o-xylene and 4-chloro-o-xylene (mass ratio: 55), heated to 187 ℃ and refluxed for 3 hours, and water produced by the reaction was removed at the time of reflux. The vacuum was turned on, the vacuum was gradually pumped to near absolute pressure and the solvent was evaporated. Cooling to normal temperature, adding 3450g of ethanol into the reaction kettle, recrystallizing for 4 hours at 70 ℃, filtering and drying in vacuum to prepare the nucleating agent.
2. And (3) crushing:
the preparation method comprises the following steps of (1) mixing a nucleating agent with polyphenylene sulfide particles with the diameter of 2-3 mm according to a mass ratio of 4: dissolving 1000 in sulfolane to obtain a 33wt% polyphenylene sulfide solution, adding water into a precipitation tank, starting stirring, starting a wet grinder to circulate water, adding the polyphenylene sulfide solution for crushing, wherein the ratio of the feeding flow rate to the water flow rate of the polyphenylene sulfide solution is 1 3 H is used as the reference value. When the polyphenylene sulfide solution is completely added, the average grain diameter of the pulverized powder is 10-30 μm, the bulk density of the wet material is 0.40g/ml, the feeding valve b is closed, and the pulverized powder is continuously pulverized for 30min, the bulk density is 0.55g/ml, the average grain diameter is 0.55g/ml5-35 μm, and the product is rod-shaped. And (3) opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
Example 5
1. Preparation of nucleating agent:
A10L reaction vessel was charged with 182.5g of 4-chlorophthalic anhydride, 38g of 1, 2-propanediol, 4410g of a mixture of 3-chloro-o-xylene and 4-chloro-o-xylene (mass ratio: 55), heated to 187 ℃ and refluxed for 3 hours, and water produced during the reaction was removed during the reflux. The vacuum was turned on, the vacuum was gradually pumped to near absolute pressure and the solvent was evaporated. Cooling to normal temperature, adding 3690g of ethanol into the reaction kettle, recrystallizing at 75 ℃ for 4 hours, filtering and drying in vacuum to prepare the nucleating agent.
2. And (3) crushing:
dissolving a nucleating agent and polyether sulfone particles with the diameter of 2-3 mm in an NMP solution according to the mass ratio of 5. Adding water into a precipitation tank, starting stirring, starting a grinder to circulate the water, adding a polymer solution for crushing, wherein the ratio of the feeding flow rate of the polyether sulfone solution to the water flow rate is 1 3 H is used as the reference value. When the polymer solution is completely added, the average particle size of the pulverized powder is 10-30 μm, the bulk density of the wet material is 0.23g/ml, the feeding valve b is closed, and after the pulverization is continued for 30min, the bulk density is 0.39g/ml, the average particle size is 8-45 μm, and the product is in a rod shape. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
Comparative example 1: non-circulating pulverizing
The nucleating agent of example 1 and polysulfone resin particles having a diameter of 2 to 3mm were dissolved in DMAC at a mass ratio of 1. Adding water into the precipitation tank, starting stirring, starting a grinding pump, and controlling the ratio of the polysulfone solution feeding flow to the water flow to be1, water flow is 5m 3 H is used as the reference value. When the polysulfone solution is precipitated and phase-changed, the crushed slurry directly enters solid-liquid separation equipment. And after the polysulfone solution is completely added and crushed, stopping the solid-liquid separation equipment and the crushing pump to finish the whole crushing process.
The test shows that the bulk density of the wet material is 0.050g/ml, and the average grain diameter is 2-5 mm.
This comparative example demonstrates that one pulverization is far less effective than multiple cycles of pulverization.
Comparative example 2: without addition of nucleating agent
Dissolving polysulfone particles with the diameter of 2-3 mm in a DMAC solution at the mass ratio of 1:1000 to obtain a 30wt% polymer solution, adding water into a precipitation tank, starting stirring, starting a grinding pump to circulate water, adding the polymer solution, grinding, wherein the ratio of the polymer solution feed flow to the water flow is 1 3 H is used as the reference value. When the polysulfone solution is added, the average particle size of the pulverized powder is 10-50 μm, the bulk density of the wet material is 0.09g/ml, the feeding valve b is closed, and after the cyclic pulverization is continued for 30min, the bulk density is 0.10g/ml, the average particle size is 5-330 μm, and the product form is irregular. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1.
This comparative example shows that the absence of the nucleating agent results in a change in the pulverized morphology of the material and a broadening of the particle size distribution after pulverization.
Comparative example 3: no enhancement effect of the added nucleating agent
The nucleating agent of example 1 and polysulfone resin particles were dissolved in DMAC at a mass ratio of 20. Adding water into the precipitation tank, starting stirring, starting a grinding pump to circulate the water, and adding polysulfone solution for grinding. The ratio of the polysulfone solution feeding flow to the water flow is 1 3 /h。
When the polysulfone solution is added, the average particle size of the pulverized powder is 10-50 μm, the bulk density of the wet material is 0.30g/ml, the feeding valve b is closed, and after the cyclic pulverization is continued for 30min, the bulk density is 0.35g/ml, the average particle size is 5-35 μm, and the product is rod-shaped. And opening a valve d, controlling the ratio of the extracted quantity to the circulating quantity to be 1. The results of this comparative example are consistent with example 1, indicating that the addition of more nucleating agent no longer has the effect of enhancing comminution.
Claims (10)
1. A nucleating agent having the formula:
wherein R 'or R' are independently benzene ring, biphenyl, acene or polyacene, polyacene and derivatives thereof, preferably benzene ring; r represents an aliphatic hydrocarbon group of 2 to 4 carbons, preferably-CH 2 -、-(CH 2 ) 2 -、-(CH 2 ) 3 -; x or Y represents halogen, preferably Cl, br, X and Y may be the same or different.
2. A process for producing a nucleating agent as claimed in claim 1, which comprises the steps of: reacting halogenated aromatic anhydride with aliphatic hydrocarbon diol.
3. The process of claim 2, wherein the molar ratio of halogenated aromatic anhydride to aliphatic hydrocarbon diol is 2.
4. The process according to claim 2 or 3, wherein the halogenated aromatic anhydride is selected from one or more of 4-chlorophthalic anhydride, 3-bromophthalic anhydride, 4-bromophthalic anhydride; the aliphatic hydrocarbon diol is one or more selected from ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol and 1, 4-butanediol.
5. A method for preparing polymer rod-like superfine powder comprises the following steps: mixing the polymer, the nucleating agent according to claim 1 and a solvent, precipitating and pulverizing.
6. The method of claim 5, comprising the steps of: mixing polymer solution of polymer, nucleating agent and solvent with inert solvent, precipitating polymer, and pulverizing into slurry to obtain polymer rod-like superfine powder.
7. Method according to claim 5 or 6, characterized in that it comprises the following steps: the settling tank with stirring, the polymer solution feeding pipe and the high-speed crushing equipment are connected to form a circulating crushing system; adding an inert solvent into a precipitation tank, circulating the inert solvent in a system after a high-speed crushing device is started, adding a polymer solution of a polymer, a nucleating agent and a solvent into the inert solvent, and crushing the mixture into slurry in the high-speed crushing device; after the feeding of the polymer solution is completed, the cyclic pulverization is maintained.
8. The method of any one of claims 5 to 7, wherein the polymer comprises one or more of an imide polymer, a sulfone polymer, a ketone polymer, a polyurethane, an aromatic polyamide, a cellulose, a fluoropolymer.
9. The process according to any one of claims 5 to 8, wherein the mass ratio of the nucleating agent to the polymer is 1.
10. The process of any one of claims 5 to 9, wherein the solvent comprises one or more of N, N-dimethylacetamide, N-methylpyrrolidone, sulfolane, dimethylsulfoxide, N-dimethylformamide, acetic acid, butyric acid; the inert solvent comprises one or more of water, ethanol, methanol isopropanol, toluene and xylene.
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