CN102532523A - Method for preparing magnetic polyamide composite material through in-situ hydrolysis - Google Patents
Method for preparing magnetic polyamide composite material through in-situ hydrolysis Download PDFInfo
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- CN102532523A CN102532523A CN2010106139611A CN201010613961A CN102532523A CN 102532523 A CN102532523 A CN 102532523A CN 2010106139611 A CN2010106139611 A CN 2010106139611A CN 201010613961 A CN201010613961 A CN 201010613961A CN 102532523 A CN102532523 A CN 102532523A
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Abstract
The invention discloses a method for preparing a magnetic polyamide composite material through in-situ hydrolysis. The method comprises the following steps of: mixing aqueous solutions of ferric salt and ferrous salt; adding an alkali solution into the mixture; reacting to obtain ferroferric oxide nanoparticles; adding a surfactant; continuously reacting to obtain modified ferroferric oxide nanoparticles; adjusting the pH value of the solution to be neutral; adding a lactam monomer; gradually heating to 250 DEG C in the reduced pressure distillation process; and performing in-situ hydrolysis bulk polymerization for 2 to 5 hours to obtain the ferroferric oxide/polyamide magnetic composite material. According to the method, the process is simple and is convenient to operate. The reaction adopts continuous in-situ polymerization, so magnetic particles are dispersed uniformly. The method is high in efficiency, low in cost and suitable for industrialized production. The obtained magnetic polyamide composite material has high industrial application value.
Description
Technical field
The present invention relates to field of magnetic material, relate in particular to a kind of in-situ hydrolysis preparation method of magnetic polyamide compoiste material.
Background technology
Polymeric amide is a kind of engineering plastics that have wide range of applications; Have price low, be prone to machine-shaping, HS, high-wearing feature, high corrosion resistance and good nerve, advantage such as anti-aging, but polymeric amide is as a kind of macromolecular material, he itself nonmagnetic; Be difficult to use it for fields such as electronic apparatus, instrument, microwave device; Can not play shielding electromagnetic wave and the effect that absorbs microwave, therefore, range of application has received corresponding restriction.
Summary of the invention
The present invention is exactly the in-situ hydrolysis preparation method that a kind of magnetic polyamide compoiste material is provided for the problem that solves above-mentioned prior art existence.
The object of the invention is realized through following technical scheme:
A kind of in-situ hydrolysis preparation method of magnetic polyamide compoiste material may further comprise the steps:
(1) is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the water and mixes with the mol ratio of metering, vacuumizes and lead to nitrogen and keep away oxygen that high-speed stirring, control water temperature are 40 ℃, dropwise add alkaline solution, make mol ratio Fe in the mixture
3+: Fe
2+: OH
-=2:1:8, solution becomes black by sorrel, is warmed up to 80 ℃ then, adds tensio-active agent, continues reaction 30-60min, the nano ferriferrous oxide particle that obtains modifying;
(2) solution that above-mentioned steps (1) is obtained is at last regulated pH value to neutral, adds the lactam monomers of metering; Mix, system is heated to 180-200 ℃ under nitrogen protection, after the complete fusion of thing to be mixed; Begin to stir, subsequently system is warming up to 250-260 ℃, pressure remains on 0.8MPa; Keep this temperature and pressure, polymerization 2-5h; The slow release of final system keeps 0.5h with balanced reaction at normal temperatures and pressures, vacuumizes 1h, removes small molecules polyreaction is carried out to accomplish polymerization, discharging to positive dirction.
Said alkaline solution is ammoniacal liquor and metal hydroxide solutions; Said metal hydroxide solutions comprises sodium hydroxide solution, potassium hydroxide solution.
Said tensio-active agent is all tensio-active agents that can modify the Z 250 particle, comprises in oleic acid, oleate, X 2073, the sodium lauryl sulphate one or more.
The add-on of said tensio-active agent is the theoretical 5-30% that generates the quality of Z 250 of step (1).
Said lactam monomers is one or more in the C4-C12 lactan, comprises in butyrolactam, hexanolactam, spicy inner formyl amine, oenantholactam or the laurolactam one or more; Said polymeric amide is a kind of homopolymer of lactam monomers or the multipolymer of several kinds of lactam monomers.
The add-on of said lactam monomers is that the theoretical quality that generates Z 250 of step (1) is the 0.1-20% of lactam monomers add-on.
Compared with prior art, the present invention has following beneficial effect:
The present invention adopts the continuous in-situ polymerization to prepare Z 250/polymeric amide magnetic composite; Aqueous solution with trivalent iron salt and divalent iron salt; In mixture, adding alkaline solution then reacts and obtains the nano ferriferrous oxide particle; Add tensio-active agent then, continue the nano ferriferrous oxide particle that reaction obtains modifying; Above-mentioned solution is regulated pH value to neutral, and the adding lactam monomers is warmed up to 250 ℃ gradually in the vacuum distillation process, carry out the in-situ hydrolysis bulk polymerization, reacts to prepare Z 250/polymeric amide magnetic composite in 2-5 hour.
Present method technology is simple, and is easy to operate, and the continuous in-situ polymerization is adopted in reaction, and magnetic particle is uniformly dispersed, and is efficient and low-cost, is fit to suitability for industrialized production, and gained magnetic polyamide compoiste material has higher industrial application value.
Embodiment
Describe the present invention in detail below in conjunction with each embodiment.
Embodiment 1
(1) with 4.7g FeCl
36H
2O and 1.7g FeCl
24H
2O is dissolved in the water and mixes, and vacuumizes logical nitrogen and keeps away oxygen, and high-speed stirring, control water temperature are 40 ℃; Dropwise add 70ml ammoniacal liquor (1mol/L), solution becomes black by sorrel, is warmed up to 80 ℃ then; Add 0.2g oleic acid, continue reaction 30min, the nano ferriferrous oxide particle that obtains modifying.
(2) solution that above-mentioned (1) is obtained is regulated PH to neutral, adds the 100g caprolactam monomer; Mix, system is heated to 180-200 ℃ under nitrogen protection; After the complete fusion of thing to be mixed, begin to stir, subsequently system is warming up to 250-260 ℃; Pressure keeps 0.8MPa, keeps this temperature and pressure, polymerization 2 hours; Final system slowly unloads and is depressed into normal temperature, under normal pressure, keeps 0.5h with balanced reaction, vacuumizes 1h, thereby removes small molecules, makes polyreaction accomplish polymerization to positive dirction, discharging.
Embodiment 2
(1) with 2.4g FeCl
36H
2O and 0.85g FeCl
24H
2O is dissolved in the water and mixes, and vacuumizes logical nitrogen and keeps away oxygen, and high-speed stirring, control water temperature are 40 ℃; Dropwise add 35ml ammoniacal liquor (1mol/L), solution becomes black by sorrel, is warmed up to 80 ℃; Add the 0.3g sodium oleate, continue reaction 40min, the nano ferriferrous oxide particle that obtains modifying.
(2) solution that above-mentioned (1) is obtained is regulated PH to neutral, adds 100g oenantholactam monomer; Mix, system is heated to 180-200 ℃ under nitrogen protection; After the complete fusion of thing to be mixed, begin to stir, subsequently system is warming up to 250-260 ℃; Pressure keeps 0.8MPa, keeps this temperature and pressure, polyase 13 hour; Final system slowly unloads and is depressed into normal temperature, under normal pressure, keeps 0.5h with balanced reaction, vacuumizes 1h, thereby removes small molecules, makes polyreaction accomplish polymerization to positive dirction, discharging.
Embodiment 3
(1) with 9.4g FeCl
36H
2O and 3.4g FeCl
24H
2O is dissolved in the water and mixes, and vacuumizes logical nitrogen and keeps away oxygen, high-speed stirring; Control water temperature is 40 ℃, dropwise adds 140ml potassium hydroxide solution (1mol/L), and solution becomes black by sorrel; Be warmed up to 80 ℃; Add the 1.0g X 2073, continue reaction 50min, the nano ferriferrous oxide particle that obtains modifying.
(2) solution that above-mentioned (1) is obtained is regulated PH to neutral, adds 100g spicy inner formyl amine monomer; Mix, system is heated to 180-200 ℃ under nitrogen protection; After the complete fusion of thing to be mixed, begin to stir, subsequently system is warming up to 250-260 ℃; Pressure keeps 0.8MPa, keeps this temperature and pressure, polymerization 4h; Final system slowly unloads and is depressed into normal temperature, under normal pressure, keeps 0.5h with balanced reaction, vacuumizes 1h, thereby removes small molecules, makes polyreaction accomplish polymerization to positive dirction, discharging.
Embodiment 4
(1) with 18.8g FeCl
36H
2O and 6.8g FeCl
24H
2O is dissolved in the water and mixes, and vacuumizes logical nitrogen and keeps away oxygen, high-speed stirring; Control water temperature is 40 ℃, dropwise adds 140ml sodium hydroxide solution (2mol/L), and solution becomes black by sorrel; Be warmed up to 80 ℃; Add 3g oleic acid, continue reaction 1 hour, the nano ferriferrous oxide particle that obtains modifying.
(2) solution that above-mentioned (1) is obtained is regulated PH to neutral, adds 100g butyrolactam monomer; Mix, system is heated to 180-200 ℃ under nitrogen protection; After the complete fusion of thing to be mixed, begin to stir, subsequently system is warming up to 250-260 ℃; Pressure keeps 0.8MPa, keeps this temperature and pressure, polymerization 5h; Final system slowly unloads and is depressed into normal temperature, under normal pressure, keeps 0.5h with balanced reaction, vacuumizes 1h, thereby removes small molecules, makes polyreaction accomplish polymerization to positive dirction, discharging.
Embodiment 5
A kind of in-situ hydrolysis preparation method of magnetic polyamide compoiste material may further comprise the steps:
(1) is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the water and mixes with the mol ratio of metering, vacuumizes and lead to nitrogen and keep away oxygen that high-speed stirring, control water temperature are 40 ℃, dropwise add alkaline solution ammoniacal liquor, make mol ratio Fe in the mixture
3+: Fe
2+: OH
-=2:1:8, solution becomes black by sorrel, is warmed up to 80 ℃ then, adds the tensio-active agent sodium lauryl sulphate, continues reaction 30min, the nano ferriferrous oxide particle that obtains modifying; Wherein the add-on of tensio-active agent is 5% of the theoretical quality that generates Z 250 of step (1);
(2) solution that above-mentioned steps (1) is obtained is at last regulated pH value to neutral, adds the laurolactam monomer of metering; Mix, system is heated to 180 ℃ under nitrogen protection, after the complete fusion of thing to be mixed; Begin to stir, subsequently system is warming up to 250 ℃, pressure remains on 0.8MPa; Keep this temperature and pressure, polymerization 2h; The slow release of final system keeps 0.5h with balanced reaction at normal temperatures and pressures, vacuumizes 1h, removes small molecules polyreaction is carried out to accomplish polymerization, discharging to positive dirction; Wherein the monomeric add-on of laurolactam does, the theoretical quality that generates Z 250 of step (1) is 0.1% of a laurolactam monomer add-on.
Embodiment 6
A kind of in-situ hydrolysis preparation method of magnetic polyamide compoiste material may further comprise the steps:
(1) is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the water and mixes with the mol ratio of metering, vacuumizes and lead to nitrogen and keep away oxygen that high-speed stirring, control water temperature are 40 ℃, dropwise add sodium hydroxide solution, make mol ratio Fe in the mixture
3+: Fe
2+: OH
-=2:1:8, solution becomes black by sorrel, is warmed up to 80 ℃ then, adds the tensio-active agent X 2073, continues reaction 60min, the nano ferriferrous oxide particle that obtains modifying; Wherein the add-on of tensio-active agent is 30% of the theoretical quality that generates Z 250 of step (1);
(2) solution that above-mentioned steps (1) is obtained is at last regulated pH value to neutral, adds the butyrolactam monomer of metering; Mix, system is heated to 200 ℃ under nitrogen protection, after the complete fusion of thing to be mixed; Begin to stir, subsequently system is warming up to 260 ℃, pressure remains on 0.8MPa; Keep this temperature and pressure, polymerization 5h; The slow release of final system keeps 0.5h with balanced reaction at normal temperatures and pressures, vacuumizes 1h, removes small molecules polyreaction is carried out to accomplish polymerization, discharging to positive dirction; Wherein the monomeric add-on of butyrolactam does, the theoretical quality that generates Z 250 of step (1) is 20% of a butyrolactam monomer add-on.
Embodiment 7
A kind of in-situ hydrolysis preparation method of magnetic polyamide compoiste material may further comprise the steps:
(1) is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the water and mixes with the mol ratio of metering, vacuumizes and lead to nitrogen and keep away oxygen that high-speed stirring, control water temperature are 40 ℃, dropwise add potassium hydroxide solution, make mol ratio Fe in the mixture
3+: Fe
2+: OH
-=2:1:8, solution becomes black by sorrel, is warmed up to 80 ℃ then, adds tensio-active agent oleic acid, continues reaction 45min, the nano ferriferrous oxide particle that obtains modifying; Wherein the add-on of tensio-active agent is 20% of the theoretical quality that generates Z 250 of step (1);
(2) solution that above-mentioned steps (1) is obtained is at last regulated pH value to neutral, adds the caprolactam monomer of metering; Mix, system is heated to 190 ℃ under nitrogen protection, after the complete fusion of thing to be mixed; Begin to stir, subsequently system is warming up to 255 ℃, pressure remains on 0.8MPa; Keep this temperature and pressure, polyase 13 .5h; The slow release of final system keeps 0.5h with balanced reaction at normal temperatures and pressures, vacuumizes 1h, removes small molecules polyreaction is carried out to accomplish polymerization, discharging to positive dirction; Wherein the add-on of caprolactam monomer does, the theoretical quality that generates Z 250 of step (1) is 10% of a caprolactam monomer add-on.
More than the disclosed several specific embodiments that are merely the application, but the application is not limited thereto, any those skilled in the art can think variation, all should drop in the application's the protection domain.
Claims (6)
1. the in-situ hydrolysis preparation method of a magnetic polyamide compoiste material is characterized in that, may further comprise the steps:
(1) is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the water and mixes with the mol ratio of metering, vacuumizes and lead to nitrogen and keep away oxygen that high-speed stirring, control water temperature are 40 ℃, dropwise add alkaline solution, make mol ratio Fe in the mixture
3+: Fe
2+: OH
-=2:1:8, solution becomes black by sorrel, is warmed up to 80 ℃ then, adds tensio-active agent, continues reaction 30-60min, the nano ferriferrous oxide particle that obtains modifying;
(2) solution that above-mentioned steps (1) is obtained is at last regulated pH value to neutral, adds the lactam monomers of metering; Mix, system is heated to 180-200 ℃ under nitrogen protection, after the complete fusion of thing to be mixed; Begin to stir, subsequently system is warming up to 250-260 ℃, pressure remains on 0.8MPa; Keep this temperature and pressure, polymerization 2-5h; The slow release of final system keeps 0.5h with balanced reaction at normal temperatures and pressures, vacuumizes 1h, removes small molecules polyreaction is carried out to accomplish polymerization, discharging to positive dirction.
2. the in-situ hydrolysis preparation method of a kind of magnetic polyamide compoiste material as claimed in claim 1 is characterized in that, said alkaline solution is ammoniacal liquor and metal hydroxide solutions; Said metal hydroxide solutions comprises sodium hydroxide solution, potassium hydroxide solution.
3. the in-situ hydrolysis preparation method of a kind of magnetic polyamide compoiste material as claimed in claim 1; It is characterized in that; Said tensio-active agent is all tensio-active agents that can modify the Z 250 particle, comprises in oleic acid, oleate, X 2073, the sodium lauryl sulphate one or more.
4. the in-situ hydrolysis preparation method of a kind of magnetic polyamide compoiste material as claimed in claim 1 is characterized in that, the add-on of said tensio-active agent is the theoretical 5-30% that generates the quality of Z 250 of step (1).
5. the in-situ hydrolysis preparation method of a kind of magnetic polyamide compoiste material as claimed in claim 1; It is characterized in that; Said lactam monomers is one or more in the C4-C12 lactan, comprises in butyrolactam, hexanolactam, spicy inner formyl amine, oenantholactam or the laurolactam one or more; Said polymeric amide is a kind of homopolymer of lactam monomers or the multipolymer of several kinds of lactam monomers.
6. the in-situ hydrolysis preparation method of a kind of magnetic polyamide compoiste material as claimed in claim 1 is characterized in that, the add-on of said lactam monomers is that the theoretical quality that generates Z 250 of step (1) is the 0.1-20% of lactam monomers add-on.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105017523A (en) * | 2015-07-29 | 2015-11-04 | 苏州荣昌复合材料有限公司 | Magnetic-adsorption nylon material |
| CN105062047A (en) * | 2015-07-29 | 2015-11-18 | 苏州荣昌复合材料有限公司 | Preparation method of magnetic adsorption nylon material |
| CN106893311A (en) * | 2015-12-18 | 2017-06-27 | 上海杰事杰新材料(集团)股份有限公司 | A kind of magnetic Nano polymer composite and preparation method thereof |
| CN110655117A (en) * | 2019-09-30 | 2020-01-07 | 天津大学 | Method for preparing ferroferric oxide with different sizes and good dispersibility |
| CN112011176A (en) * | 2019-05-29 | 2020-12-01 | 北京服装学院 | Magnetic polyamide, preparation method thereof and magnetic fiber obtained by using magnetic polyamide |
| CN112876674A (en) * | 2021-03-17 | 2021-06-01 | 滨州学院 | Method for preparing polyamide microspheres through in-situ hydrolytic ring opening |
| CN113045781A (en) * | 2021-03-19 | 2021-06-29 | 北京化工大学 | Method for preparing high-strength cast nylon product |
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| CN101885915A (en) * | 2010-08-11 | 2010-11-17 | 哈尔滨工业大学 | Method for preparing magnetic ferroferric oxide/conductive polyaniline light-weight composite hollow microspheres |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105017523A (en) * | 2015-07-29 | 2015-11-04 | 苏州荣昌复合材料有限公司 | Magnetic-adsorption nylon material |
| CN105062047A (en) * | 2015-07-29 | 2015-11-18 | 苏州荣昌复合材料有限公司 | Preparation method of magnetic adsorption nylon material |
| CN106893311A (en) * | 2015-12-18 | 2017-06-27 | 上海杰事杰新材料(集团)股份有限公司 | A kind of magnetic Nano polymer composite and preparation method thereof |
| CN112011176A (en) * | 2019-05-29 | 2020-12-01 | 北京服装学院 | Magnetic polyamide, preparation method thereof and magnetic fiber obtained by using magnetic polyamide |
| CN110655117A (en) * | 2019-09-30 | 2020-01-07 | 天津大学 | Method for preparing ferroferric oxide with different sizes and good dispersibility |
| CN112876674A (en) * | 2021-03-17 | 2021-06-01 | 滨州学院 | Method for preparing polyamide microspheres through in-situ hydrolytic ring opening |
| CN113045781A (en) * | 2021-03-19 | 2021-06-29 | 北京化工大学 | Method for preparing high-strength cast nylon product |
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Denomination of invention: Method for preparing magnetic polyamide composite material through in-situ hydrolysis Effective date of registration: 20191202 Granted publication date: 20140910 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |
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