CN114702699A - Method for producing polyamide powder and polyamide powder - Google Patents
Method for producing polyamide powder and polyamide powder Download PDFInfo
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- CN114702699A CN114702699A CN202210364537.0A CN202210364537A CN114702699A CN 114702699 A CN114702699 A CN 114702699A CN 202210364537 A CN202210364537 A CN 202210364537A CN 114702699 A CN114702699 A CN 114702699A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/122—Pulverisation by spraying
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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
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses polyamide powder and a preparation method thereof, and relates to the technical field of preparation of high polymer materials. Spraying a polyamide melt with the viscosity of 500-10000 mPa.s under the pressure of 0.6-5 MPa, and blowing and atomizing the polyamide melt by using inert gas to obtain initial polyamide powder. The viscosity of the movement of the polyamide melt is controlled to control the polyamide melt to spray and discharge at a lower molecular weight, the viscosity of the polyamide melt with the lower molecular weight is low, the surface tension is low, the sprayed polyamide melt is blown and cut into powder mist by inert gas at a high speed, and the initial polyamide powder with uniform particle size distribution and smooth surface can be obtained, so that a new method is provided for the preparation of the polyamide powder.
Description
Technical Field
The invention relates to the technical field of preparation of high polymer materials, and particularly relates to a preparation method of polyamide powder and the polyamide powder.
Background
The polyamide material, also known as nylon, is the first synthetic fiber appearing in the world, has good wear resistance and wide application, and is commonly used for preparing various fabrics, medical supplies, engineering plastics and the like.
At present, two methods are mainly used for industrially producing polyamide powder, namely a mechanical crushing method and a solvent method. Mechanical comminution is generally referred to as cryogenic comminution, the comminution being carried out by reducing the polyamide to an extremely low temperature using liquid nitrogen. However, the polyamide powder obtained by this method often has the phenomena of uneven particle size distribution, irregular particle surface, edges and corners, poor fluidity and the like, and the application of the polyamide powder is limited. The solvent method generally adopts an organic solvent to dissolve the polyamide at high temperature and high pressure, and polyamide powder with uniform particle size distribution can be obtained by a spray drying or solution extraction method. The solvent used in the solvent method usually adopts alcohols or other organic solvents with high toxicity, the alcohols are flammable and explosive under high temperature condition, the requirements on the process and equipment are very strict, and the potential safety hazard of production also exists; organic solvents are toxic, mostly have pungent odor, are harmful to the health of workers, and are not environment-friendly.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of polyamide powder and the polyamide powder.
The invention is realized in the following way:
in a first aspect, the present invention provides a method for preparing a polyamide powder, comprising spraying a polyamide melt having a viscosity of 500 to 10000mpa.s at a pressure of 0.6 to 5MPa, and purging and atomizing the polyamide melt with an inert gas to obtain an initial polyamide powder.
In a second aspect, the present invention provides a polyamide powder obtained by the method according to any one of the above embodiments, wherein the particle size of the polyamide powder is 15 to 300 μm.
The invention has the following beneficial effects:
the invention provides polyamide powder and a preparation method thereof, wherein the viscosity of the movement of a polyamide melt is controlled to control the polyamide melt to spray and discharge at a lower molecular weight, and the sprayed polyamide melt is in a powder-like state by inert gas purging due to the low molecular weight, the viscosity of the polyamide melt in a molten state and the small surface tension, so that the initial polyamide powder with uniform particle size distribution and smooth surface can be obtained, and a new method is provided for the preparation of the polyamide powder. The initial polyamide powder provides excellent initial morphology for the finished polyamide powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Polyamide material, also known as nylon, is the first synthetic fiber appearing in the world, has good wear resistance and wide application, and is commonly used for preparing various fabrics, medical supplies, engineering plastics and the like.
At present, two methods are mainly used for industrially producing polyamide powder, namely a mechanical crushing method and a solvent method. The mechanical pulverization method is generally referred to as cryogenic pulverization, and pulverization is carried out by lowering the temperature of polyamide to an extremely low level using liquid nitrogen. However, the polyamide powder obtained by this method often has the phenomena of uneven particle size distribution, irregular particle surface, edges and corners, poor fluidity and the like, and the application of the polyamide powder is limited. The solvent method generally adopts an organic solvent to dissolve the polyamide at high temperature and high pressure, and polyamide powder with uniform particle size distribution can be obtained by a spray drying or solution extraction method. The solvent used in the solvent method usually adopts alcohols or other organic solvents with high toxicity, the alcohols are flammable and explosive under high temperature condition, the requirements on the process and equipment are very strict, and the potential safety hazard of production also exists; organic solvents are toxic, mostly have pungent odor, are harmful to the health of workers, and are not environment-friendly. Therefore, how to prepare polyamide powder with regular particle shape and surface and safe and simple preparation method is a technical problem which needs to be solved for a long time in the field.
In a first aspect, the present invention provides a method for preparing a polyamide powder, comprising spraying a polyamide melt having a viscosity of 500 to 10000mpa.s at a pressure of 0.6 to 5MPa, and purging and atomizing the polyamide melt with an inert gas to obtain an initial polyamide powder.
The viscosity of the movement of the polyamide melt is controlled to control the molecular weight of the polyamide melt during discharging, the polyamide melt is discharged by spraying when the molecular weight of the polyamide melt is lower, the viscosity and the surface tension of the polyamide melt in a molten state are low, the sprayed polyamide melt is blown by inert gas to be in a powder-like state, and the initial polyamide powder with uniform particle size distribution and smooth surface can be obtained, so that a novel method is provided for preparing the polyamide powder. The initial polyamide powder provides excellent initial morphology for the finished polyamide powder.
The method not only retains the advantages of good particle shape and good fluidity of the polyamide powder prepared by the solvent method, but also solves the problem of potential safety hazard caused by the organic solvent added in the preparation process of the solvent method, and provides a new idea for the preparation of the polyamide powder.
In an alternative embodiment, the polyamide melt with the viscosity of 500 to 10000mpa.s is obtained by testing the viscosity of the polyamide melt with an online viscometer, and in other embodiments, the polyamide melt can be detected by other methods as long as the polyamide melt can be detected within the viscosity range of 500 to 10000mpa.s, and the detection method is not limited by the invention.
Preferably, the viscosity is controlled within the range of 500-10000 mPa.s, so that the polyamide melt has a lower molecular weight, the subsequent spraying is convenient, and if the viscosity of the polyamide melt is higher than the range, the particle size of the initial polyamide powder formed after spraying is uneven, the particle surface is irregular, and the application range is limited.
Preferably, the viscosity of the polyamide melt is 500 to 5000mPa.s, more preferably 500 to 3000 mPa.s.
In an alternative embodiment, the injecting comprises: keeping the pressure of the polyamide melt at 0.6-5 MPa, and ejecting the polyamide melt through a discharge die hole.
Preferably, the diameter of the nozzle of the discharge die hole is 0.05-0.3 mm, the diameter of the nozzle of the discharge die hole determines the particle size of the polyamide powder, and the particle size of the polyamide powder obtained by controlling the diameter of the nozzle within the range is uniform and has good particle fineness.
Preferably, the nozzle is a laval nozzle, and the laval nozzle has a special structure, so that the air flow speed changes along with the change of the cross section area of the nozzle during the spraying process, the air flow is sprayed at high speed, and the spraying speed can even reach supersonic speed. In other embodiments, the nozzle may be a conventional nozzle, as long as it can eject the polyamide melt at a high speed.
In an optional embodiment, the polyamide melt is sprayed out from the discharging die hole, and due to the low viscosity and the small surface tension of the low molecular weight polyamide melt, the low molecular weight polyamide melt cannot maintain the original shape and is broken into small polyamide particles after being sprayed out from the discharging die hole at a high speed, and inert gas is used for high-speed blowing and cutting for further pulverization, so that initial polyamide powder with small particle size and uniform particles is obtained. The preferred melt has a higher jet velocity after passing through a Laval nozzle, the melt can be rapidly broken and cracked after being expanded through an outlet, and the particle size of the obtained polyamide powder is finer after being cut by inert gas at a high speed.
Meanwhile, in order to ensure the surface uniformity of the polyamide powder, the method also comprises the step of heating the inert gas before blowing and atomizing the polyamide melt by using the inert gas. During the cutting process of the heated inert gas, the residual temperature in the gas can make the cutting surface of the polyamide melt tend to be in a molten state, and the surface of the obtained initial polyamide powder is regular.
Preferably, the temperature of the heated inert gas is 240-400 ℃. For example, the temperature after the inert gas is heated may be 240 ℃, 260 ℃, 280 ℃, 300 ℃, 320 ℃, 340 ℃, 360 ℃, 380 ℃ and 400 ℃.
Preferably, the inert gas comprises at least one of nitrogen, argon, carbon dioxide, more preferably the inert gas is nitrogen.
In an alternative embodiment, in order to ensure the surface regularity of the initial polyamide powder, the step of rapidly cooling and solidifying the polyamide melt after the step of blowing and atomizing the polyamide melt with the inert gas to obtain the initial polyamide powder. Because the cutting surface is in a micro-molten state after the polyamide melt is cut by the high-temperature inert gas, the cut polyamide melt needs to be cooled in time to prevent the deformation of particles.
Preferably, the initial polyamide powder has an intrinsic viscosity of 0.1 to 0.5 dL/g. For example, the initial polyamide powder may have an intrinsic viscosity of 0.1dL/g, 0.2dL/g, 0.3dL/g, 0.4dL/g, and 0.5 dL/g. Controlling the viscosity of the initial polyamide powder within the above range and controlling the polyamide discharge at a lower molecular weight helps to reduce the particle size of the polyamide powder, more preferably the particle size of the initial polyamide powder is 0.1 to 0.3 dL/g.
In an alternative embodiment, the polyamide melt is prepared by mixing the diacid, diamine, and third monomer with water and polymerizing.
Preferably, the polymerization reaction comprises the steps of uniformly mixing the dibasic acid, the diamine and the third monomer with water, raising the temperature to 200-280 ℃, keeping the pressure at 0.6-5 MPa, and discharging the added solvent water and water vapor generated in the reaction process.
In an alternative embodiment, the diacid includes at least one of an aromatic diacid including at least one of terephthalic acid, isophthalic acid, naphthalene dicarboxylic acid, and isophthalic acid or an aliphatic diacid including at least one of a C4-C15 aliphatic diacid;
the diamine comprises at least one of C4-C15 aliphatic diamine.
The third monomer is at least one of caprolactam, 5-aminopentanoic acid, 9-aminononanoic acid, 10-aminodecanoic acid, 11-aminoundecanoic acid and 12-aminododecanoic acid;
preferably, in order to ensure the smooth progress of the reaction, the addition amount of the third monomer is 5 to 80 percent of the total weight of the raw materials, and the total mole number of the diamine and the diacid is the same.
In an alternative embodiment, it also comprises solid-phase tackification of the starting polyamide powder and two screenings to obtain a polyamide powder.
In an optional embodiment, the temperature of solid phase tackifying is 170-280 ℃ and the time is 1-36 h.
In a second aspect, the present invention provides a polyamide powder produced by the production method according to any one of the preceding embodiments. Wherein the particle size of the polyamide powder is 15 to 300 μm. Preferably, the particle size of the polyamide powder is 15 to 200 μm.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This example provides a polyamide powder having a particle size of 50 to 100 μm. The preparation method of the polyamide powder comprises the following steps:
s101, preparing a polyamide melt: 2490g (15mol) of terephthalic acid, 1740g (15mol) of hexamethylenediamine and 1695g (15mol) of caprolactam are weighed according to the weight ratio and mixed evenly with 3000g of water, 2, the temperature is raised to 240 ℃, the pressure is kept at 2MPa, polymerization reaction occurs, and solvent water added during feeding and water vapor generated in the reaction process are continuously discharged during the polymerization reaction.
S102, testing the viscosity of the polyamide melt to be 1500mPa.s by using an online viscometer, keeping the reaction pressure to be 2MPa, and discharging the polyamide melt through a discharging die hole in a spraying mode. The nozzle of the discharging die hole is a Laval nozzle with the diameter of 0.2 mm.
S103, heating nitrogen to 300 ℃, blowing and atomizing the polyamide melt sprayed from the discharge die hole, and then rapidly cooling and solidifying to obtain initial polyamide powder, wherein the intrinsic viscosity of the initial polyamide powder is 0.15 dL/g.
S104, solid-phase thickening of the initial polyamide powder is performed to increase the molecular weight of the initial polyamide powder. And screening the polyamide powder subjected to solid-phase tackifying twice, removing polyamide powder particles with the particle size of more than 100 microns by using a 160-mesh filter screen, and removing polyamide powder particles with the particle size of less than 50 microns by using a 270-mesh filter screen to obtain polyamide powder with the particle size of 50-100 microns.
Wherein the solid-phase viscosity increasing temperature is 240 ℃, the time is 4 hours, and the final inherent viscosity of the polyamide powder is 0.8 dL/g.
Example 2
This example provides a polyamide powder having a particle size of 100 to 200. mu.m. The preparation method of the polyamide powder comprises the following steps:
s101, preparing a polyamide melt: 2490g (15mol) of terephthalic acid, 2580g (15mol) of decamethylene diamine, 2805g (15mol) of 10-aminodecanoic acid and 3000g of water are weighed according to the weight ratio and uniformly mixed, the temperature is raised to 220 ℃, the pressure is kept at 1.5MPa, polymerization reaction occurs, and solvent water added during feeding and water vapor generated in the reaction process are continuously discharged during the polymerization reaction.
S102, testing the viscosity of the polyamide melt to be 2000mPa.s by using an online viscometer, keeping the reaction pressure to be 1.5MPa, and discharging the polyamide melt through a discharging die hole in an injection mode. The nozzle of the discharging die hole is a Laval nozzle with the diameter of 0.3 mm.
S103, heating nitrogen to 300 ℃, blowing and atomizing the polyamide melt sprayed from the discharge die hole, and then rapidly cooling and solidifying to obtain initial polyamide powder, wherein the intrinsic viscosity of the initial polyamide powder is 0.1 dL/g.
S104, solid-phase thickening of the initial polyamide powder is performed to increase the molecular weight of the initial polyamide powder. And then sieving the polyamide powder subjected to solid-phase tackification twice, removing polyamide powder particles with the particle size of more than 100 micrometers by using a 70-mesh filter screen, and removing polyamide powder particles with the particle size of less than 50 micrometers by using a 160-mesh filter screen to obtain polyamide powder with the particle size of 100-200 micrometers.
Wherein the temperature of solid phase tackifying is 180 ℃, the time is 24h, and the final inherent viscosity of the polyamide powder is 0.9 dL/g.
Example 3
This example provides a polyamide powder having a particle size of 15 to 50 μm. The preparation method of the polyamide powder comprises the following steps:
s101, preparing a polyamide melt: 2490g (15mol) of terephthalic acid, 1740g (mol) of hexamethylenediamine, 2260g (20mol) of caprolactam and 3000g of water are weighed according to the weight ratio, mixed uniformly, the temperature is raised to 250 ℃, the pressure is kept at 3.5MPa, polymerization reaction occurs, and solvent water added during feeding and water vapor generated in the reaction process are continuously discharged during the polymerization reaction.
S102, testing the viscosity of the polyamide melt to be 1000mPa.s by using an online viscometer, keeping the reaction pressure to be 3.5MPa, and discharging the polyamide melt through a discharging die hole in an injection mode. The nozzle of the discharging die hole is a Laval nozzle with the diameter of 0.1 mm.
S103, heating nitrogen to 350 ℃, blowing and atomizing the polyamide melt sprayed from the discharge die hole, and then rapidly cooling and solidifying to obtain initial polyamide powder, wherein the intrinsic viscosity of the initial polyamide powder is 0.2 dL/g.
S104, solid-phase thickening of the initial polyamide powder is performed to increase the molecular weight of the initial polyamide powder. And screening the polyamide powder subjected to solid-phase tackifying twice, removing polyamide powder particles with the particle size of more than 500 microns by using a 300-mesh filter screen, and removing polyamide powder particles with the particle size of less than 15 microns by using a 800-mesh filter screen to obtain polyamide powder with the particle size of 15-50 microns.
Wherein the temperature of solid phase tackifying is 220 ℃, the time is 8h, and the final inherent viscosity of the polyamide powder is 0.85 dL/g.
Comparative example 1
This comparative example provides a polyamide powder which was prepared in a manner similar to that of example 1, except that the viscosity of the polyamide melt was 20000mPa.s, the initial intrinsic viscosity was 0.6dL/g, the sprayed polyamide melt was filamentous, and the filamentous polyamide was obtained after cutting with a nitrogen purge, and no polyamide powder could be formed.
Comparative example 2
This comparative example provides a polyamide powder, which was prepared in a manner similar to that of example 2, except that the spraying pressure of the polyamide melt was 0.3MPa, the system pressure was too low, the material was difficult to stably spray, and was sometimes slowly flowed out and formed into droplets, and after cutting with nitrogen purge, the particle size was difficult to control, the particle size difference was large, the maximum particle size was up to 1000 μm or more, and the particle size difference was up to 2000 μm or more.
Comparative example 3
This comparative example provides a polyamide powder having a starting material composition similar to that of example 3, except that a conventional cryogenic mechanical pulverization process was used to prepare the polyamide powder, specifically as follows:
cooling polyamide resin PA6T-6 to below-80 ℃ by using liquid nitrogen, crushing by using a liquid nitrogen ultralow-temperature freezing crusher, and then screening to obtain polyamide powder with the particle size of 50-100 mu m. The polyamide crushing process is slow, the energy consumption is high, the polyamide needs to be reduced to the extremely low temperature, and the obtained polyamide powder has edges and corners through microscope observation and is poor in flowability.
Test example 1
The polyamide powders prepared in examples 1 to 3 and comparative examples 1 to 3 were tested by the following methods:
polyamide powder flowability test method: according to the test of the fluidity of the metal powder in the national standard GB/T1482-2010 and the standard funnel method, the termination time T of the complete flowing-out of the powder is recorded, the shorter the time is, the better the fluidity is, and the detection results are shown in Table 1.
Method for testing surface edges and corners of polyamide powder: taking a proper amount of polyamide powder, spreading the polyamide powder to be thin, placing the polyamide powder on a glass sheet, covering another glass sheet on a kettle, flattening the glass sheet into a thin sheet, observing the polyamide powder under a microscope to determine whether the polyamide powder has edges and corners or not, wherein the powder cannot be overlapped as much as possible under the microscope, and the detection results are shown in table 1.
TABLE 1 Property parameters of the Polyamide powders
| Fluidity t/s | Surface corner angle | Whether to be powdered or not | |
| Example 1 | 62 | Is free of | Is that |
| Example 2 | 68 | Is free of | Is that |
| Example 3 | 75 | Is free of | Is that |
| Comparative example 1 | - | - | Whether or not |
| Comparative example 2 | - | - | Whether or not |
| Comparative example 3 | 108 | Most have edges and corners | Is that |
In summary, the polyamide powder prepared by the preparation method provided by the invention has at least the following advantages:
the viscosity of the movement of the polyamide melt is controlled to control the molecular weight of the polyamide melt during discharging, the polyamide melt is discharged by spraying when the molecular weight of the polyamide melt is lower, and the polyamide melt in a molten state has low viscosity and low surface tension, so that the sprayed polyamide melt is blown into powder mist by inert gas, the initial polyamide powder with uniform particle size distribution and smooth surface can be obtained, and a new method is provided for preparing the polyamide powder. The initial polyamide powder provides excellent initial morphology for obtaining the final polyamide powder product.
In addition, the polyamide powder prepared by the method has uniform particle size, high yield, excellent solvent resistance and temperature resistance, does not use an organic solvent, does not need crushing and grinding, is simple and convenient in preparation method, and is environment-friendly. The method also enables the preparation of a semi-aromatic polyamide powder.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of polyamide powder is characterized by comprising the steps of spraying a polyamide melt with the viscosity of 500-10000 mPa.s under the pressure of 0.6-5 MPa, and blowing and atomizing the polyamide melt by using inert gas to obtain initial polyamide powder.
2. The production method according to claim 1, wherein the polyamide melt having a viscosity of 500 to 10000mPa.s is obtained by measuring the viscosity of the polyamide melt using an in-line viscometer.
3. The method of manufacturing according to claim 1, wherein the spraying includes: keeping the pressure of the polyamide melt at 0.6-4 MPa, and ejecting the polyamide melt through a discharge die hole;
preferably, the diameter of a nozzle of the discharging die hole is 0.05-0.3 mm;
preferably, the nozzle is a laval nozzle.
4. The preparation method of claim 1, wherein before the step of purging and atomizing the polyamide melt with the inert gas, the step of heating the inert gas is further included, and the temperature of the inert gas after heating is 240-400 ℃;
preferably, the inert gas comprises at least one of nitrogen, argon, carbon dioxide.
5. The method according to claim 1, wherein the step of cooling and solidifying the polyamide melt after the step of blowing and atomizing the polyamide melt with inert gas to obtain the initial polyamide powder;
preferably, the initial polyamide powder has an intrinsic viscosity of 0.1 to 0.5 dL/g.
6. The preparation method of any one of claims 2 to 5, wherein the preparation method of the polyamide melt comprises the steps of mixing a dibasic acid, a diamine and a third monomer with water to perform a polymerization reaction;
preferably, the polymerization reaction comprises the steps of uniformly mixing the dibasic acid, the diamine and the third monomer with water, raising the temperature to 200-280 ℃, keeping the pressure at 0.6-5 MPa, and discharging the added solvent water and water vapor generated in the reaction process.
7. The method of claim 6, wherein the dibasic acid comprises at least one of an aromatic dibasic acid or an aliphatic dibasic acid; preferably, the aromatic dibasic acid comprises at least one of terephthalic acid, isophthalic acid, naphthalene dicarboxylic acid, and isophthalic acid; the aliphatic dibasic acid comprises at least one of C4-C15 aliphatic dibasic acid;
the diamine comprises at least one of C4-C15 aliphatic diamine;
the third monomer is at least one of caprolactam, 5-aminopentanoic acid, 9-aminononanoic acid, 10-aminodecanoic acid, 11-aminoundecanoic acid and 12-aminododecanoic acid;
preferably, the addition amount of the third monomer is 5-80% of the total weight of the raw materials, and the total moles of the diamine and the diacid are the same.
8. The method according to any one of claims 2 to 5, further comprising subjecting the initial polyamide powder to solid-phase adhesion and sieving; preferably, the sieving is performed twice.
9. The preparation method according to claim 8, wherein the temperature of the solid phase adhesion is 170-280 ℃ and the time is 1-36 h.
10. A polyamide powder produced by the production method according to any one of claims 1 to 9;
the particle size of the polyamide powder is 15-300 mu m.
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| CN107849241A (en) * | 2015-07-29 | 2018-03-27 | 帝斯曼知识产权资产管理有限公司 | The polymer composition for preparing the method for polymer composition and can be obtained by methods described |
| CN112020381A (en) * | 2018-04-25 | 2020-12-01 | 阿科玛法国公司 | Loose wax powder and method for producing such powder |
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2022
- 2022-04-07 CN CN202210364537.0A patent/CN114702699A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5244984A (en) * | 1989-01-20 | 1993-09-14 | Daicel Huls Ltd. | Process for producing polymer powder |
| JPH0570598A (en) * | 1991-09-17 | 1993-03-23 | Daicel Huels Ltd | Manufacture of cosmetic polyamide powder |
| CN101437870A (en) * | 2006-05-04 | 2009-05-20 | Uhde英万达·费希尔公开股份有限公司 | Method for the continuous production of polyamide granules |
| CN103649172A (en) * | 2011-07-05 | 2014-03-19 | 巴斯夫欧洲公司 | Solid particles, containing lactam, activator, and catalyst, method for producing said solid particles, and use of said solid particles |
| CN107849241A (en) * | 2015-07-29 | 2018-03-27 | 帝斯曼知识产权资产管理有限公司 | The polymer composition for preparing the method for polymer composition and can be obtained by methods described |
| CN112020381A (en) * | 2018-04-25 | 2020-12-01 | 阿科玛法国公司 | Loose wax powder and method for producing such powder |
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