CN114773590A - Preparation method of high-quality polyamide - Google Patents
Preparation method of high-quality polyamide Download PDFInfo
- Publication number
- CN114773590A CN114773590A CN202210565714.1A CN202210565714A CN114773590A CN 114773590 A CN114773590 A CN 114773590A CN 202210565714 A CN202210565714 A CN 202210565714A CN 114773590 A CN114773590 A CN 114773590A
- Authority
- CN
- China
- Prior art keywords
- mixture
- quality polyamide
- compound
- quality
- putting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a preparation method of high-quality polyamide, which comprises the steps of providing pentanediamine, lithium nitrate and adipate compounds, putting the pentanediamine, the lithium nitrate and the adipate compounds into a stirring tank to form mixed powder, carrying out wet ball milling for 12 hours, drying and taking out a mixture; putting the mixture, caprolactam, sodium hypophosphite and water into a reaction kettle to complete the third polymerization; discharging the materials, cooling and dicing to obtain high-quality polyamide wet chips; and (3) putting the wet slices into an extraction drying device, extracting for 36h by boiling water at 100 ℃, and drying for 36h by high-purity nitrogen at 135 ℃ to obtain the high-quality polyamide. According to the invention, through premixing the pentanediamine, the lithium nitrate and the adipate compound, then putting the mixture into a reaction kettle for polymerization reaction with the caprolactam, the sodium hypophosphite and the water, the high-quality polyamide wet slice is obtained, and the high-quality polyamide is obtained through extraction, so that the product has high strength and good quality.
Description
Technical Field
The invention belongs to the technical field of high-quality fibers, and particularly relates to a preparation method of high-quality polyamide.
Background
Polyamide, commonly known as nylon, is a general name of thermoplastic resins having a repeating amide group- [ NHCO ] -in a molecular main chain, and is first developed by dupont in the united states and industrialized in 1939, and has been widely used because of its good comprehensive properties and easy processing. The main species are polyamide 6 and polyamide 66, and in addition polyamide 11, 12, etc., and also various copolymers. Polyamide 6/66 copolymers are of interest because of their high strength and high elasticity.
The high-quality polyamide fiber mainly utilizes the technologies of melt spinning, dry spinning, zone stretching heat setting and the like, has great requirements on military and civilian aspects, and mainly refers to the fiber with the tensile breaking strength of more than 6.0 cN/dtex. According to the prior art, the tensile strength of domestic high-strength polyimide 6 fibers can rarely reach more than 10.0cN/dtex, and the strength variation coefficient and the tensile elongation variation coefficient of the high-strength polyimide 6 fibers can not meet the standard requirements and have poor quality.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing high-quality polyamide, which is used to avoid the trouble of insufficient strength and poor quality of the conventional polyamide.
In order to solve the technical problems, the invention discloses a preparation method of high-quality polyamide, which comprises the following steps:
step a, providing a pentanediamine compound, a lithium nitrate compound and an adipate compound with a molar ratio of 1:0.5:1, putting the pentanediamine compound, the lithium nitrate compound and the adipate compound into a stirring tank to form mixed powder, carrying out wet ball milling for 12 hours, and taking out a mixture after drying;
b, putting the mixture, caprolactam, sodium hypophosphite and water into a reaction kettle, replacing the mixture with nitrogen for 3-5 times, heating the mixture to the temperature of 110-;
c, continuously heating to 220 ℃, keeping the pressure at 0.2-1.8MPa for 2.5 hours, and finishing secondary polymerization;
d, slowly discharging gas until the pressure is 0.1MPa, simultaneously heating to 270 ℃, vacuumizing to-0.05 MPa, and keeping for half an hour to finish polymerization for three times;
discharging materials, cooling and dicing to obtain high-quality polyamide wet chips;
and f, putting the wet slices into an extraction drying device, extracting for 36h by boiling water at 100 ℃, and drying for 36h by high-purity nitrogen at 135 ℃ to obtain the high-quality polyamide.
According to an embodiment of the invention, wherein the adipate compound is selected from one or more of hexamethylenediamine, adipic acid, terephthalic acid, isophthalic acid, sebacic acid, decanediamine, dodecanedioic acid, dodecanediamine, undecanolactam, dodecanolactam.
According to an embodiment of the present invention, in the step b, the mixture comprises caprolactam, sodium hypophosphite and water in a ratio of 850: 150: 1: 120.
according to an embodiment of the present invention, in the steps b to d, the temperature increase rate is 5 ℃/min.
According to an embodiment of the invention, the purity of the mixture in the step a is more than or equal to 99.5%.
Compared with the prior art, the invention can obtain the following technical effects:
the high-quality polyamide wet chip is obtained by premixing pentanediamine, lithium nitrate and adipate compound, then putting the mixture into a reaction kettle for polymerization reaction with caprolactam, sodium hypophosphite and water, and the high-quality polyamide wet chip is obtained by extraction, so that the product has high strength and good quality.
Of course, it is not necessary for any one product to achieve all of the above-described technical effects simultaneously in order to practice the present invention.
Detailed Description
The following detailed description will be provided to illustrate embodiments of the present invention, so that the implementation process of the present invention, which applies technical means to solve technical problems and achieve technical effects, can be fully understood and implemented.
The invention discloses a preparation method of high-quality polyamide, which comprises the following steps:
step a, providing a pentanediamine compound, a lithium nitrate compound and an adipate compound with a molar ratio of 1:0.5:1, putting the pentanediamine compound, the lithium nitrate compound and the adipate compound into a stirring tank to form mixed powder, carrying out wet ball milling for 12 hours, and taking out a mixture after drying;
b, putting the mixture, caprolactam, sodium hypophosphite and water into a reaction kettle, replacing the mixture with nitrogen for 3-5 times, heating the mixture to the temperature of 110-;
c, continuously heating to 220 ℃, keeping the pressure at 0.2-1.8MPa for 2.5 hours, and finishing secondary polymerization;
d, slowly discharging gas until the pressure is 0.1MPa, simultaneously heating to 270 ℃, vacuumizing to-0.05 MPa, and keeping for half an hour to finish the polymerization for three times;
discharging materials, cooling and dicing to obtain high-quality polyamide wet chips;
and f, putting the wet slices into an extraction drying device, extracting for 36h by boiling water at 100 ℃, and drying for 36h by high-purity nitrogen at 135 ℃ to obtain the high-quality polyamide.
In one embodiment of the present invention, pentanediamine, lithium nitrate and adipate compound are mixed to form a high quality nylon 56 salt, wherein lithium nitrate can relatively increase the purity of the mixture, thereby improving the quality of the product. And then putting the mixture, caprolactam, sodium hypophosphite and water into a reaction kettle for polymerization, continuously controlling the temperature and the pressure, continuously reacting, discharging wet polyamide slices, and finally extracting and drying to obtain a finished product.
Further wherein the adipate compound is selected from one or more of hexamethylenediamine, adipic acid, terephthalic acid, isophthalic acid, sebacic acid, decamethylenediamine, dodecanedioic acid, dodecanediamine, undecanolactam, and dodecanolactam.
And furthermore, in the step b, the mixture comprises caprolactam, sodium hypophosphite and water with the proportion of 850: 150: 1: 120.
furthermore, in the steps b to d, the temperature rise rate is 5 ℃/min, the temperature is slowly controlled, and the reaction sufficiency is improved.
Furthermore, the purity of the mixture in the step a is more than or equal to 99.5 percent, and the purity and the high quality of the product are ensured.
In conclusion, the high-quality polyamide wet chip is obtained by premixing the pentanediamine, the lithium nitrate and the adipate compound, then putting the mixture into a reaction kettle with the caprolactam, the sodium hypophosphite and the water for polymerization reaction, and the high-quality polyamide wet chip is obtained by extraction, so that the product has high strength and good quality.
The foregoing description shows and describes several preferred embodiments of the invention, but as aforementioned, it is to be understood that the invention is not limited to the forms disclosed herein, and is not to be construed as excluding other embodiments, and that the invention is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of high-quality polyamide is characterized by comprising the following steps:
providing a pentanediamine compound, a lithium nitrate compound and an adipate compound with a molar ratio of 1:0.5:1, putting the pentanediamine compound, the lithium nitrate compound and the adipate compound into a stirring tank to form mixed powder, performing wet ball milling for 12 hours, and taking out a mixture after drying;
b, putting the mixture, caprolactam, sodium hypophosphite and water into a reaction kettle, replacing the mixture with nitrogen for 3-5 times, heating to the temperature of 110-;
c, continuously heating to 220 ℃, keeping the pressure at 0.2-1.8MPa for 2.5 hours, and finishing secondary polymerization;
d, slowly discharging gas until the pressure is 0.1MPa, simultaneously heating to 270 ℃, vacuumizing to-0.05 MPa, and keeping for half an hour to finish the polymerization for three times;
discharging materials, cooling and dicing to obtain high-quality polyamide wet chips;
and f, putting the wet slices into an extraction drying device, extracting for 36h by boiling water at 100 ℃, and drying for 36h by high-purity nitrogen at 135 ℃ to obtain the high-quality polyamide.
2. The method for producing high-quality polyamide according to claim 1, wherein the adipate compound is one or more selected from the group consisting of hexamethylenediamine, adipic acid, terephthalic acid, isophthalic acid, sebacic acid, decamethylenediamine, dodecanedioic acid, dodecamethylenediamine, undecanolactam and dodecanolactam.
3. The method for preparing high-quality polyamide according to claim 1, wherein the mixture in step b comprises caprolactam, sodium hypophosphite and water in a ratio of 850: 150: 1: 120.
4. the method for producing high-quality polyamide according to claim 1, wherein the temperature increase rate in the steps b to d is 5 ℃/min.
5. The method for preparing high-quality polyamide according to claim 1, wherein the purity of the mixture in step a is not less than 99.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210565714.1A CN114773590A (en) | 2022-05-24 | 2022-05-24 | Preparation method of high-quality polyamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210565714.1A CN114773590A (en) | 2022-05-24 | 2022-05-24 | Preparation method of high-quality polyamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114773590A true CN114773590A (en) | 2022-07-22 |
Family
ID=82408332
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210565714.1A Withdrawn CN114773590A (en) | 2022-05-24 | 2022-05-24 | Preparation method of high-quality polyamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114773590A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449069A (en) * | 2021-06-09 | 2022-12-09 | 上海凯赛生物技术股份有限公司 | Copolyamide resin, copolyamide fiber, and preparation methods and applications thereof |
| CN116200036A (en) * | 2023-04-04 | 2023-06-02 | 江苏林泉汽车装饰件有限公司 | Automobile interior trim part material with high heat resistance |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250433A (en) * | 2017-12-19 | 2018-07-06 | 浙江恒逸锦纶有限公司 | A kind of PA6-56 copolymeric materials and preparation method thereof |
-
2022
- 2022-05-24 CN CN202210565714.1A patent/CN114773590A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250433A (en) * | 2017-12-19 | 2018-07-06 | 浙江恒逸锦纶有限公司 | A kind of PA6-56 copolymeric materials and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449069A (en) * | 2021-06-09 | 2022-12-09 | 上海凯赛生物技术股份有限公司 | Copolyamide resin, copolyamide fiber, and preparation methods and applications thereof |
| CN116200036A (en) * | 2023-04-04 | 2023-06-02 | 江苏林泉汽车装饰件有限公司 | Automobile interior trim part material with high heat resistance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114773590A (en) | Preparation method of high-quality polyamide | |
| CN107337792B (en) | Melting point-controllable copolymerized nylon powder material and preparation method thereof | |
| CN102356113B (en) | Method for making polyamide | |
| CN107177903B (en) | Blended fiber, preparation method thereof and fabric containing blended fiber | |
| CN101899152B (en) | Preparation of titanium dioxide additive in nylon-6 continuous polymerization production process | |
| CN107267109B (en) | Polyesteramide hot melt adhesive and preparation method thereof | |
| CN104162625B (en) | A kind of binder for casting and preparation method thereof | |
| CN108017779B (en) | Polyester easy to dye and preparation method thereof | |
| CN104862826B (en) | Preparation method of PIPD/PBO (poly(dihydroxyphenylene pyridobisimidazole)/poly-p-phenylene ben-zobisthiazole) blend fiber | |
| JP2014528018A5 (en) | ||
| CN107022076A (en) | A kind of preparation method of the deep dye section of polyamide fibre 6 | |
| CN109265678B (en) | Polyamide resin, preparation method thereof and molded product | |
| US10683407B2 (en) | Process for preparing polyamide granules and uses | |
| CN114573805A (en) | Preparation method of high-barrier transparent flame-retardant copolymerized nylon | |
| CN108503825B (en) | Preparation method of polyamide and prepared polyamide resin | |
| CN111364117B (en) | Preparation method of cationic easy-to-dye polyester amide fiber | |
| CN113968965A (en) | Semi-aromatic polyamide and preparation method and application thereof | |
| CN107778477A (en) | A kind of preparation method of low molecule amount polycaprolactam | |
| TWI554547B (en) | Deeply Dyed Polyamide and Its Manufacturing Method | |
| CN109957108B (en) | Polyesteramide hot melt adhesive and preparation method thereof | |
| CN115651191B (en) | Method for preparing semi-aromatic polyamide and semi-aromatic polyamide prepared by method | |
| CN105348580A (en) | Preparation method of middle tire combinations of balls | |
| CN105131280A (en) | Halogen-free flame-retardant co-polymerized polyamide 66 resin and preparation method thereof | |
| CN108570147A (en) | A kind of 6 coloured slice continuous production device of polyamide fibre and production method | |
| US5696227A (en) | Process for the batchwise preparation of polylaurolactam |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20220722 |