CN105062047A - Preparation method of magnetic adsorption nylon material - Google Patents
Preparation method of magnetic adsorption nylon material Download PDFInfo
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- CN105062047A CN105062047A CN201510454626.4A CN201510454626A CN105062047A CN 105062047 A CN105062047 A CN 105062047A CN 201510454626 A CN201510454626 A CN 201510454626A CN 105062047 A CN105062047 A CN 105062047A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention provides a preparation method of a magnetic adsorption nylon material. The preparation method comprises the following steps: step one, adding iron chloride and ferrous chloride into a glass container, stirring, at the same time, adding a sodium hydroxide solution to adjust the pH value, allowing the solution to stand still for one hour, adding ethyl orthosilicate, heating the solution for 2 to 3 hours, cooling to the room temperature, sucking out the obtained products from the solution by a magnet, washing the products by clean water until the pH value is reduced to the neutral range so as to obtain ferroferric oxide nano particles; step two, adding the ferroferric oxide nano particles obtained in the step one into a hydrochloric acid solution, carrying out ultrasonic and magnetic separation, washing, adding sodium citrate, then adding ammonia liquor, then stirring to gradually dissolve out precipitate, and washing the precipitate by distilled water to neutrality. The provided preparation method enhances the water absorbing performance of nylon material, strengthens the adsorption performance, and reduces the water absorption of nylon material. Moreover, the nylon fibers are evenly distributed, the nylon strength is strengthened, and the nylon material is enabled to have a magnetic adsorption function.
Description
Technical field
The present invention relates to the field of macromolecule modified material preparation method, especially relate to a kind of preparation method of magnetic absorption nylon material.
Background technology
Nylon 6 (PA6) is one of most important kind in nylon series product, has the features such as wear-resistant self-lubricating, oil resistant, acid and alkali-resistance and processing fluidity are good.The good mechanical and physical performance of PA6 and superior cost performance, become a kind of purposes engineering plastics very widely.But PA6 water-absorbent is large, poor dimensional stability, molding shrinkage are high, the defect such as have that low temperature impact strength is not good, toughness is not enough under drying regime, creep-resistant property is poor, particularly the modulus of pure PA6 is lower, limit its application in some fields, for making PA6 play a role, necessary to its modification.
Summary of the invention
A kind ofly can produce the nylon material with magnetic absorption function for preparing, the present invention proposes a kind of preparation method of magnetic absorption nylon material, comprising the following steps:
Step one: get iron(ic) chloride and iron protochloride is added in Glass Containers, stirs, adds sodium hydroxide solution simultaneously, regulator solution pH value, leaves standstill after 1 hour, adds tetraethoxy, carry out heating 2-3 hour to solution, be cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to neutral, obtain ferriferrous oxide nano-particle;
Step 2: the ferriferrous oxide nano-particle obtained in step one is placed in hydrochloric acid soln, carries out ultrasonic Magneto separate, washing, is adding Trisodium Citrate, then is adding ammoniacal liquor, then stirring, separating out throw out gradually in solution, be washed with distilled water to neutrality;
Step 3: add after getting hexanolactam melting in reactor, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Step 4: get PA6 and ferriferrous oxide nano-particle, drying 24 hours at 100 DEG C, coordinate forcing machine, temperature is between 230 DEG C-250 DEG C, and extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
Preferably, in step one, the mass ratio of iron(ic) chloride and iron protochloride is 1:1.
Preferably, the mass ratio in step 2 in ferriferrous oxide nano-particle and hydrochloric acid soln is 2:3-7.
Preferably, in described step 2, the mass ratio of ammoniacal liquor and total solution is: 1:2-4.
Preferably, the ratio of PA6 and ferriferrous oxide nano-particle is 1-6:1-5.
The preparation method of the magnetic absorption nylon material that the present invention proposes has following beneficial effect: the present invention is by adding polymer adsorbing material Fe304SiO2, add nylon material water-absorbent strong, increase adsorptive power, reduce the water-intake rate of material, nylon fiber is evenly distributed, intensity enhancing, and make nylon material have magnetic absorption function.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.
Embodiment 1
Get 15ml iron(ic) chloride and 15ml iron protochloride is added in Glass Containers, stir, add 2mol/L sodium hydroxide solution simultaneously, regulator solution pH value, to 10-11, leaves standstill after 1 hour, adds 2.83ml tetraethoxy, heating is carried out 2 hours to solution, is being cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to 7, obtain ferriferrous oxide nano-particle;
Get 10g ferriferrous oxide nano-particle and be placed in 50ml hydrochloric acid soln, carry out ultrasonic Magneto separate, washing, add the sodium citrate solution 5ml of 1mol/L, add 18ml ammoniacal liquor again, stir again, in solution, separate out throw out gradually, be washed with distilled water to neutrality;
Add in reactor after getting the melting of 10g hexanolactam, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Get the PA6 arrived in above-mentioned steps and ferriferrous oxide nano-particle mixes according to the ratio of 2:3, at 100 DEG C dry 24 hours, coordinate forcing machine, temperature is between 230 DEG C, extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
Embodiment 2
Get 15ml iron(ic) chloride and 15ml iron protochloride is added in Glass Containers, stir, add 3mol/L sodium hydroxide solution simultaneously, regulator solution pH value, to 10-11, leaves standstill after 1 hour, adds 5.6ml tetraethoxy, heating is carried out 3 hours to solution, is being cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to 7, obtain ferriferrous oxide nano-particle;
Get 10g ferriferrous oxide nano-particle and be placed in 60ml hydrochloric acid soln, carry out ultrasonic Magneto separate, washing, add the sodium citrate solution 5ml of 1mol/L, add 32.5ml ammoniacal liquor again, stir again, in solution, separate out throw out gradually, be washed with distilled water to neutrality;
Add in reactor after getting the melting of 10g hexanolactam, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Get the PA6 arrived in above-mentioned steps and ferriferrous oxide nano-particle mixes according to the ratio of 1:2, at 100 DEG C dry 24 hours, coordinate forcing machine, temperature is between 240 DEG C, extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
Embodiment 3
Get 15ml iron(ic) chloride and 15ml iron protochloride is added in Glass Containers, stir, add 3mol/L sodium hydroxide solution simultaneously, regulator solution pH value, to 10-11, leaves standstill after 1 hour, adds 1.69ml tetraethoxy, heating is carried out 3 hours to solution, is being cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to 7, obtain ferriferrous oxide nano-particle;
Get 10g ferriferrous oxide nano-particle and be placed in 60ml hydrochloric acid soln, carry out ultrasonic Magneto separate, washing, add the sodium citrate solution 5ml of 1mol/L, add 32.5ml ammoniacal liquor again, stir again, in solution, separate out throw out gradually, be washed with distilled water to neutrality;
Add in reactor after getting the melting of 10g hexanolactam, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Get the PA6 arrived in above-mentioned steps and ferriferrous oxide nano-particle mixes according to the ratio of 1:2, at 100 DEG C dry 24 hours, coordinate forcing machine, temperature is between 250 DEG C, extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
Embodiment 4
Get 15ml iron(ic) chloride and 15ml iron protochloride is added in Glass Containers, stir, add 3mol/L sodium hydroxide solution simultaneously, regulator solution pH value, to 10-11, leaves standstill after 1 hour, adds 1.69ml tetraethoxy, heating is carried out 3 hours to solution, is being cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to 7, obtain ferriferrous oxide nano-particle;
Get 10g ferriferrous oxide nano-particle and be placed in 60ml hydrochloric acid soln, carry out ultrasonic Magneto separate, washing, add the sodium citrate solution 5ml of 1mol/L, add 32.5ml ammoniacal liquor again, stir again, in solution, separate out throw out gradually, be washed with distilled water to neutrality;
Add in reactor after getting the melting of 10g hexanolactam, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Get the PA6 arrived in above-mentioned steps and ferriferrous oxide nano-particle mixes according to the ratio of 6:5, at 100 DEG C dry 24 hours, coordinate forcing machine, temperature is between 240 DEG C, extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
The magnetic absorption nylon material of aforesaid method is put into the solution containing 10ml/L mercury ion, places 2 minutes, detect the mercury ion content of surplus solution; And detect the pulling force characteristic of magnetic absorption nylon material.
To be apparent for those skilled in the art to the multiple amendment of embodiment, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. a preparation method for magnetic absorption nylon material, is characterized in that, comprises the following steps:
Step one: get iron(ic) chloride and iron protochloride is added in Glass Containers, stirs, adds sodium hydroxide solution simultaneously, regulator solution pH value, leaves standstill after 1 hour, adds tetraethoxy, carry out heating 2-3 hour to solution, be cooled to room temperature; Use magnet by products therefrom sucking-off from solution, use clear water to rinse to pH value to neutral, obtain ferriferrous oxide nano-particle;
Step 2: the ferriferrous oxide nano-particle obtained in step one is placed in hydrochloric acid soln, carries out ultrasonic Magneto separate, washing, is adding Trisodium Citrate, then is adding ammoniacal liquor, then stirring, separating out throw out gradually in solution, be washed with distilled water to neutrality;
Step 3: add after getting hexanolactam melting in reactor, under high pure nitrogen protection, temperature, pressure control to be polymerized 10 hours under 265 DEG C and 3 ~ 6atm respectively, and namely polymerisate obtains product P A6 after pelletizing, distillation poach, drying;
Step 4: get PA6 and ferriferrous oxide nano-particle, drying 24 hours at 100 DEG C, coordinate forcing machine, temperature is between 230 DEG C-250 DEG C, and extruding rotating speed is 60r/min, and the magnetic absorption nylon material of final system, carries out cooling pelletizing.
2. the preparation method of magnetic absorption nylon material according to claim 1, is characterized in that, in step one, the mass ratio of iron(ic) chloride and iron protochloride is 1:1.
3. the preparation method of magnetic absorption nylon material according to claim 1, is characterized in that, the mass ratio in step 2 in ferriferrous oxide nano-particle and hydrochloric acid soln is 2:3-7.
4. the preparation method of magnetic absorption nylon material according to claim 3, is characterized in that, in described step 2, the mass ratio of ammoniacal liquor and total solution is: 1:2-4.
5. the preparation method of magnetic absorption nylon material according to claim 1, is characterized in that, the ratio of PA6 and ferriferrous oxide nano-particle is 1-6:1-5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510454626.4A CN105062047A (en) | 2015-07-29 | 2015-07-29 | Preparation method of magnetic adsorption nylon material |
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| CN201510454626.4A CN105062047A (en) | 2015-07-29 | 2015-07-29 | Preparation method of magnetic adsorption nylon material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017214742A1 (en) * | 2016-06-13 | 2017-12-21 | 杨磊 | Method for preparing magnetic polyamide acid nano-composite fibre |
| CN109054364A (en) * | 2018-07-11 | 2018-12-21 | 桐城市新瑞建筑工程有限公司 | A kind of magnetism nylon material and preparation method thereof |
| CN111785961A (en) * | 2020-06-02 | 2020-10-16 | 杭州电子科技大学 | Porous ferroferric oxide film/multilayer graphene composite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04342736A (en) * | 1991-05-20 | 1992-11-30 | Motoo Takayanagi | Production of glass-containing aramid film |
| CN102477220A (en) * | 2010-11-23 | 2012-05-30 | 合肥杰事杰新材料股份有限公司 | Magnetic nylon microspheres with controllable particle size and preparation method thereof |
| CN102532523A (en) * | 2010-12-30 | 2012-07-04 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing magnetic polyamide composite material through in-situ hydrolysis |
| CN104231615A (en) * | 2014-09-28 | 2014-12-24 | 唐贵凤 | Magnetic nylon composite material and preparation method thereof |
-
2015
- 2015-07-29 CN CN201510454626.4A patent/CN105062047A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04342736A (en) * | 1991-05-20 | 1992-11-30 | Motoo Takayanagi | Production of glass-containing aramid film |
| CN102477220A (en) * | 2010-11-23 | 2012-05-30 | 合肥杰事杰新材料股份有限公司 | Magnetic nylon microspheres with controllable particle size and preparation method thereof |
| CN102532523A (en) * | 2010-12-30 | 2012-07-04 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing magnetic polyamide composite material through in-situ hydrolysis |
| CN104231615A (en) * | 2014-09-28 | 2014-12-24 | 唐贵凤 | Magnetic nylon composite material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 吴江渝 等: "磁性二氧化硅纳米粒子的制备及性能", 《武汉工程大学学报》 * |
| 张可喜 等: "《材料合成与制备研究》", 30 April 2014 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017214742A1 (en) * | 2016-06-13 | 2017-12-21 | 杨磊 | Method for preparing magnetic polyamide acid nano-composite fibre |
| CN109054364A (en) * | 2018-07-11 | 2018-12-21 | 桐城市新瑞建筑工程有限公司 | A kind of magnetism nylon material and preparation method thereof |
| CN111785961A (en) * | 2020-06-02 | 2020-10-16 | 杭州电子科技大学 | Porous ferroferric oxide film/multilayer graphene composite material and preparation method thereof |
| CN111785961B (en) * | 2020-06-02 | 2021-07-23 | 杭州电子科技大学 | Porous ferroferric oxide film/multilayer graphene composite material and preparation method thereof |
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