CN107815102A - A kind of preparation method of the anhydrite powder composite of nylon 6 of anodizing modified carbon fiber enhancing - Google Patents

A kind of preparation method of the anhydrite powder composite of nylon 6 of anodizing modified carbon fiber enhancing Download PDF

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Publication number
CN107815102A
CN107815102A CN201711054689.6A CN201711054689A CN107815102A CN 107815102 A CN107815102 A CN 107815102A CN 201711054689 A CN201711054689 A CN 201711054689A CN 107815102 A CN107815102 A CN 107815102A
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China
Prior art keywords
nylon
carbon fiber
modified
anhydrite powder
anodizing
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Pending
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CN201711054689.6A
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Chinese (zh)
Inventor
宋庆海
康志国
苏华
刘志国
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Taishan Gypsum (tongling) Co Ltd
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Taishan Gypsum (tongling) Co Ltd
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Priority to CN201711054689.6A priority Critical patent/CN107815102A/en
Publication of CN107815102A publication Critical patent/CN107815102A/en
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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
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/10—Silicon-containing compounds
    • 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
    • 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
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • 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
    • C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

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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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of the anhydrite powder composite of nylon 6 of anodizing modified carbon fiber enhancing, it is characterized in that, by anhydrite powder after high-temperature calcination and surface modified active reason, for modification of nylon 6, using stearic acid dry method modification wollastonite fibre, anodizing modified carbon fiber as reinforcing material, the anhydrite powder composite of nylon 6/ is prepared；It is put into after nylon 6 is dried with modified filler anhydrite powder in high-speed mixer, oxidation modification carbon fiber, the mixing of modified silicon ash mineral wool are put into again, through double screw extruder extruding pelletization, standard specimen is injected into through injection machine after gained pellet is dried, that is, obtains the composite.

Description

A kind of nylon 6- anhydrite powder composites of anodizing modified carbon fiber enhancing Preparation method
Technical field
The present invention relates to gypsum field, and in particular to a kind of nylon 6- anhydrite of anodizing modified carbon fiber enhancing The preparation method of powder composite material.
Background technology
Gypsum is processed to it and gypsum gel, gypsum building products etc. is made as one of three big gel rubber materials
Material, extensive use is obtained in industry, building and medical material field etc..Although in its mechanical property
Aspect, there is higher compression strength, but its rupture strength and tensile strength are poor.The defects of these aspects, limits
The application field of gypsum material is made, the defects of in order to improve gypsum in this respect, generally use adding of fiber comes
Strengthen the mechanical property of gypsum.The one kind of anhydrite as inorganic filler, there is sound insulation, heat-insulated, fire-retardant, wearability is good etc. Feature, had a wide range of applications in fields such as polymer matrix composites, and its surface hydrophilicity and its and matrix material The shortcomings that poor compatibility, seriously restricts its application process.Therefore, its surface hydrophilicity is changed, to strengthen it compatible with matrix material Property and interface binding power be beneficial to giving full play to for its performance, to anhydrite carry out activation process be solve this problem it is effective Approach.
The content of the invention
The present invention solves the technical problem of providing, a kind of nylon 6- of anodizing modified carbon fiber enhancing is hard The preparation method of gypsum powder composite material, the composite prepared according to this method have good waterproof water resistance.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of preparation method of the nylon 6- anhydrite powder composites of anodizing modified carbon fiber enhancing, its feature exist In preparing for nylon 6- anhydrite powder composites is as follows：
After 90-100 parts nylon 6 is dried into 6-8h at 95-97 DEG C, it is put into modified filler anhydrite powder in high-speed mixer, Oxidation modification carbon fiber, the mixing of modified silicon ash mineral wool are put into again, and through double screw extruder extruding pelletization, gained pellet is existed 7-8h is dried at 94-96 DEG C, then standard specimen is injected into through injection machine, that is, obtains the composite.
Wherein,（1）The activation process of modified filler anhydrite powder is as follows：
By 0.2-0.3 part silane couplers KH560 by volume 1:50 are dispersed in solvent absolute ethyl alcohol, obtain mixed solution；
15-20 part anhydrite powders are placed in 95-105 DEG C of baking oven and dry 1-2h, then are placed in 690-710 DEG C of Muffle furnace high temperature calcining 1-2h, then put into high-speed mixer, mixed solution spraying is added thereto mixing 10-20min, 78-82 DEG C is warming up to and changes Property 1-2h after, in 95-105 DEG C of baking oven dry 1-2h, obtain modified filler anhydrite powder；
Wherein, particle diameter is that the anhydrite powder ratio of 3000/2000/1500/800 mesh is 10/2/5/2-5.
（2）The method of anodizing modified carbon fiber is as follows：
0.5-0.6mol/L electrolyte phosphoric acid solution is prepared, in a cell electrolysis processing 0.2-0.4 part carbon fibers, after electrolysis It is clear through deionized water, 7-8h then is dried at 115-125 DEG C, oxidation modification carbon fiber is made；Wherein, carbon fiber particle diameter is grown Spend for 15mm.
（3）Preparing for modified silicon ash mineral wool is as follows：
0.02-0.05 part modifying agent stearic acid is added into 2-3 part wollastonite fibres, under the conditions of 74-76 DEG C at stirring reaction 15-17min is managed, is ground after cooling, obtains dry method modification wollastonite fibre；
The temperature of extrusion zone is respectively 200-205 DEG C from hopper to head, 210-220 DEG C, 210-230 DEG C, 220-235 DEG C, 230-235 DEG C, 225-230 DEG C, screw speed 180-200r/min；Injection temperature is followed successively by 215- from charge door to nozzle 220℃、225-230℃、235-240℃、245-250℃。
The present invention reaction mechanism and have the beneficial effect that：
Wollastonite fibre is handled through stearic acid dry method modification, surface roughness is improved, strengthens its boundary with plaster matrix Face combination degree, improve composite property；By carbon fiber, electrolysis is handled in electrolyte phosphoric acid solution, the carbon after anodic oxidation Fiber surface is coarse, and oxygen-containing functional group increase, its is hydrophilic to sexually revise, and is spiked into the performance that composite can be improved in gypsum；Will Anhydrite powder is after high-temperature calcination and the processing of surface modified active, for modification of nylon 6, with dry method modification wollastonite fibre, oxygen Change modified carbon fiber is reinforcing material, prepares the anhydrite powder composite of nylon 6/；High-temperature calcination removes the knot in anhydrite powder Brilliant water, coupling agent KH560 improves its dispersiveness by covalent bond keyed to the surface of anhydrite particle after surface modification treatment, For modification of nylon 6, interfacial bonding property is good between the two, can improve the mechanical property and heat endurance of composite；It is modified fine The addition of dimension can improve the mechanical property and water resistance of composite.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of preparation method of the nylon 6- anhydrite powder composites of anodizing modified carbon fiber enhancing, its feature It is, preparing for nylon 6- anhydrite powder composites is as follows：
After 90-100 parts nylon 6 is dried into 6-8h at 95-97 DEG C, it is put into modified filler anhydrite powder in high-speed mixer, Oxidation modification carbon fiber, the mixing of modified silicon ash mineral wool are put into again, and through double screw extruder extruding pelletization, gained pellet is existed 7-8h is dried at 94-96 DEG C, then standard specimen is injected into through injection machine, that is, obtains the composite.
Wherein,（1）The activation process of modified filler anhydrite powder is as follows：
By 0.2-0.3 part silane couplers KH560 by volume 1:50 are dispersed in solvent absolute ethyl alcohol, obtain mixed solution；
15-20 part anhydrite powders are placed in 95-105 DEG C of baking oven and dry 1-2h, then are placed in 690-710 DEG C of Muffle furnace high temperature calcining 1-2h, then put into high-speed mixer, mixed solution spraying is added thereto mixing 10-20min, 78-82 DEG C is warming up to and changes Property 1-2h after, in 95-105 DEG C of baking oven dry 1-2h, obtain modified filler anhydrite powder；
Wherein, particle diameter is that the anhydrite powder ratio of 3000/2000/1500/800 mesh is 10/2/5/2-5.
（2）The method of anodizing modified carbon fiber is as follows：
0.5-0.6mol/L electrolyte phosphoric acid solution is prepared, in a cell electrolysis processing 0.2-0.4 part carbon fibers, after electrolysis It is clear through deionized water, 7-8h then is dried at 115-125 DEG C, oxidation modification carbon fiber is made；Wherein, carbon fiber particle diameter is grown Spend for 15mm.
（3）Preparing for modified silicon ash mineral wool is as follows：
0.02-0.05 part modifying agent stearic acid is added into 2-3 part wollastonite fibres, under the conditions of 74-76 DEG C at stirring reaction 15-17min is managed, is ground after cooling, obtains dry method modification wollastonite fibre；
The temperature of extrusion zone is respectively 200-205 DEG C from hopper to head, 210-220 DEG C, 210-230 DEG C, 220-235 DEG C, 230-235 DEG C, 225-230 DEG C, screw speed 180-200r/min；Injection temperature is followed successively by 215- from charge door to nozzle 220℃、225-230℃、235-240℃、245-250℃。

Claims (6)

1. a kind of preparation method of the nylon 6- anhydrite powder composites of anodizing modified carbon fiber enhancing, its feature exist In by anhydrite powder after high-temperature calcination and the processing of surface modified active, for modification of nylon 6, with stearic acid dry method modification silicon Grey mineral wool, anodizing modified carbon fiber are reinforcing material, prepare the anhydrite powder composite of nylon 6/；Nylon 6 is dried Be put into after dry with modified filler anhydrite powder in high-speed mixer, then put into oxidation modification carbon fiber, modified silicon ash mineral wool mixes Close, through double screw extruder extruding pelletization, be injected into standard specimen through injection machine after gained pellet is dried, that is, obtain described multiple Condensation material.
2. the nylon 6- anhydrite powder composites that a kind of anodizing modified carbon fiber strengthens according to claim 1 Preparation method, it is characterised in that preparing for the anhydrite powder composite of nylon 6/ is as follows：
After 90-100 parts nylon 6 is dried into 6-8h at 95-97 DEG C, it is put into modified filler anhydrite powder in high-speed mixer, Oxidation modification carbon fiber, the mixing of modified silicon ash mineral wool are put into again, and through double screw extruder extruding pelletization, gained pellet is existed 7-8h is dried at 94-96 DEG C, then standard specimen is injected into through injection machine, that is, obtains the composite.
3. the nylon 6- anhydrite powder composites that a kind of anodizing modified carbon fiber strengthens according to claim 2 Preparation method, it is characterised in that the activation process of modified filler anhydrite powder is as follows：
By 0.2-0.3 part silane couplers KH560 by volume 1:50 are dispersed in solvent absolute ethyl alcohol, obtain mixed solution；
15-20 part anhydrite powders are placed in 95-105 DEG C of baking oven and dry 1-2h, then are placed in 690-710 DEG C of Muffle furnace high temperature calcining 1-2h, then put into high-speed mixer, mixed solution spraying is added thereto mixing 10-20min, 78-82 DEG C is warming up to and changes Property 1-2h after, in 95-105 DEG C of baking oven dry 1-2h, obtain modified filler anhydrite powder；
Wherein, particle diameter is that the anhydrite powder ratio of 3000/2000/1500/800 mesh is 10/2/5/2-5.
4. the nylon 6- anhydrite powder composites that a kind of anodizing modified carbon fiber strengthens according to claim 2 Preparation method, it is characterised in that the method for anodizing modified carbon fiber is as follows：
0.5-0.6mol/L electrolyte phosphoric acid solution is prepared, in a cell electrolysis processing 0.2-0.4 part carbon fibers, after electrolysis It is clear through deionized water, 7-8h then is dried at 115-125 DEG C, oxidation modification carbon fiber is made；Wherein, carbon fiber particle diameter is grown Spend for 15mm.
5. the nylon 6- anhydrite powder composites that a kind of anodizing modified carbon fiber strengthens according to claim 2 Preparation method, it is characterised in that preparing for modified silicon ash mineral wool is as follows：
0.02-0.05 part modifying agent stearic acid is added into 2-3 part wollastonite fibres, under the conditions of 74-76 DEG C at stirring reaction 15-17min is managed, is ground after cooling, obtains dry method modification wollastonite fibre；
Wherein wollastonite fibre draw ratio is 15:1st, granularity is 800 mesh, mixing speed 1000-1500r/min.
6. the nylon 6- anhydrite powder composites that a kind of anodizing modified carbon fiber strengthens according to claim 2 Preparation method, it is characterised in that the temperature of extrusion zone is respectively 200-205 DEG C, 210-220 DEG C, 210-230 from hopper to head DEG C, 220-235 DEG C, 230-235 DEG C, 225-230 DEG C, screw speed 180-200r/min；Injection temperature is from charge door to spray Mouth is followed successively by 215-220 DEG C, 225-230 DEG C, 235-240 DEG C, 245-250 DEG C.
CN201711054689.6A 2017-11-01 2017-11-01 A kind of preparation method of the anhydrite powder composite of nylon 6 of anodizing modified carbon fiber enhancing Pending CN107815102A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104059358A (en) * 2014-06-11 2014-09-24 金发科技股份有限公司 Flame-retardant thermoplastic polyamide composition, and preparation method and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104059358A (en) * 2014-06-11 2014-09-24 金发科技股份有限公司 Flame-retardant thermoplastic polyamide composition, and preparation method and application thereof

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Application publication date: 20180320