CN106189214A - A kind of preparation method of high intensity MC nylon modified fibre composite base material - Google Patents
A kind of preparation method of high intensity MC nylon modified fibre composite base material Download PDFInfo
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- CN106189214A CN106189214A CN201610621070.8A CN201610621070A CN106189214A CN 106189214 A CN106189214 A CN 106189214A CN 201610621070 A CN201610621070 A CN 201610621070A CN 106189214 A CN106189214 A CN 106189214A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—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
- 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
- C08G69/16—Preparatory processes
-
- 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
- C08K2201/001—Conductive additives
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses the preparation method of a kind of high intensity MC nylon modified fibre composite base material, the method includes: the graphene oxide of preparation high oxidation degree；It is modified graphene oxide processing；Preparation one prepares high intensity MC nylon composite junction brick.The mechanical property that the present invention uses asphalt base carbon fiber to enhance material can be adsorbed and the harmful gas of removing in tail gas and dust material, the advantage that obtained MC nylon combination property is good greatly.It is adjuvant with the use of plasticizer, age resistor, self-control modified hydrotalcite, attapulgite clay, nano titanium oxide, nano-cerium oxide, accelerator etc.; component raw material prepares reasonable science; the composition added not only can have its material protected of effective guarantee nonflammable, and the too high burning of temperature also will not produce harmful gas；With the brucite used in the market, there is the most high temperature resistant, fire prevention, fire-retardant advantage.
Description
Technical field
The present invention relates to the preparation method of a kind of high intensity MC nylon modified fibre composite base material, particularly to a kind of MC Buddhist nun
The preparation method of dragon/modified graphene oxide nano composite material.
Background technology
Monomer cast nylon (MC nylon) is one of current most widely used engineering plastics, and it has low cost, high yield, height
The advantages such as reaction rate and good mechanical performance, are widely used in preparing bearing, gear, pulley etc., especially prepare
The large-scale device can not prepared by compression moulding or extrusion molding, MC nylon progressively replaces some metal materials in a lot of fields,
Such as copper, aluminum, steel and ferrum etc..But, compared with metal material, it is high that MC nylon there are still elastic modelling quantity, and low-temperature flexibility is poor,
The shortcomings such as impact strength is on the low side, and dimensional stability is bad, make the application of MC nylon be somewhat limited, domestic for this
External enhancing, the aspect such as toughness reinforcing conduct extensive research.
Implant is mainly incorporated into polymerization forming in caprolactam monomer by the activeness and quietness modification of MC nylon, main
Implant has inorganic filler, fibrous material, elastomeric material and nano material.Traditional modifying agent and method mostly can only be improved
MC nylon performance in a certain respect, and to a certain extent to weaken other performance as cost.Such as add mineral powder, toughness reinforcing
While often make intensity reduce；Toughness is the most generally made to reduce during fiberglass reinforced；And often add graft copolymerization elastic body toughening
It is with the valuable rigidity of expendable material, dimensional stability, thermostability as cost, carries it is therefore necessary to find a kind of modifying agent
The combination property of high MC nylon.
Summary of the invention
The present invention solves that above-mentioned technical problem provides a kind of preparation method preparing high intensity MC nylon composite junction brick,
The method preparation simplicity, technique is simple, and it is good that the one obtained prepares high intensity MC nylon composite junction brick combination property, is protecting
On the premise of holding MC nylon hot strength and hardness, significantly improve the impact strength of MC nylon.
The technical scheme is that a kind of preparation method preparing high intensity MC nylon composite junction brick, including following step
Rapid:
A. the graphite oxide of high oxidation degree is prepared；
B. the graphite oxide using cetyl trimethylammonium bromide to obtain step a is modified processing, and to changing of obtaining
Property graphite oxide use and ultrasonic obtain graphene oxide；
C. situ aggregation method is used to prepare MC nylon/modified graphene oxide nano composite material；
D. add non-halogenated organophosphinate, hexamethylenetetramine, tri-methyl-amyl triethoxysilane, conductive mica powder,
Conductive nano graphite powder, the trimer of polyisocyanates, polytetrafluoroethylene fibre, nanoparticle active agent, plasticizer, age resistor, from
Modified hydrotalcite processed, attapulgite clay, nano titanium oxide, nano-cerium oxide, accelerator；
E. after remaining component being pulverized and mixed, standby after crossing 100-200 mesh screen；Stir prepared high temperature 90-100 DEG C
Base material；
F. by compound, base material being extruded into adobe by vacuum extruder, the vacuum of vacuum extruder is 1.0-1.8Mpa,
Extrusion pressure is 15-20Mpa；
Each component proportion described is: graphene oxide 5-10 weight portion, non-halogenated organophosphinate 5-7 part, six methines
Tetramine 8-10 part, tri-methyl-amyl triethoxysilane 2-4 part, conductive mica powder 0.3-0.5 weight portion, conductive nano graphite powder
0.2-0.4 weight portion, the trimer 0.8-1 weight portion of polyisocyanates, polytetrafluoroethylene fibre 1-2 weight portion, nano active
Agent 20-30 weight portion, plasticizer 2-8 weight portion, age resistor 1-5 weight portion, self-control modified hydrotalcite 2-6 weight portion, attapulgite
Stone clay 10-18 weight portion, nano titanium oxide 8-12 weight portion, nano-cerium oxide 6-14 weight portion, accelerator 2-6 weight
Part；
G. by after the adobe of step (f) under field conditions (factors) dry in the sun 15 days at a temperature of 700 DEG C sinter molding；Base material is put into
In Mechanical processing of casting machine, first adding pressurizing melting on vulcanizing press at foundry goods, melt temperature is 160-190 DEG C, after constant temperature 3-5h certainly
So cooling.
Described nanoparticle active agent is the compositions of MgO, Al2O3, Si3N4, BN；
The preparation method of described self-control modified hydrotalcite is: a certain amount of magnesium aluminum-hydrotalcite is scattered in the deionized water of de-CO2
In make serosity after the NaH2PO4 2H2O of excess is dissolved in water institute wiring solution-forming is poured slowly in serosity, heated and stirred is also used
Acetic acid regulation PH to about 3.7, reacts 3 hours under reflux temperature, after natural cooling, with the deionized water wash of de-CO2
Product also filters until filtrate PH=7, is then dried to obtain self-control modified hydrotalcite.
Step a is prepared high oxidation degree graphite oxide include: added by concentrated sulphuric acid in graphite, through-20 DEG C ~-10 DEG C
Low temperature stirs 5-12 hour, then after 0 DEG C ~ 5 DEG C stirrings 5-12 hour, addition potassium permanganate carries out oxidation reaction and aoxidized
Graphite solution.
Step b use cetyl trimethylammonium bromide (CTAB) graphene oxide modification is included: in step a
In obtain graphite oxide solution is directly added into CTAB, CTAB and graphite oxide flocculated and modified-reaction obtains modified oxidized
Graphite solution.
Graphite with the mass ratio of CTAB is: 10:1 ~ 20:1, and graphite with the mass ratio of potassium permanganate is: 1:1 ~ 1:5.
In step c, use situ aggregation method to prepare MC nylon/modified graphene oxide nano composite material and include: incite somebody to action oneself
Lactams is heated to 70 DEG C-100 DEG C and extremely melts, and the modified graphene oxide solution that mass fraction is 0.05% ~ 5% joins oneself
Adding a certain amount of catalyst in lactams fused solution, decompression distillation removes by-product in 30-60 minute, is eventually adding a certain amount of
Activator (TDI), pours in preheated mould after stirring rapidly, react 1-4 hour at 80-150 DEG C.
Described catalyst is sodium hydroxide, and described activator is 2,4 toluene diisocyanate.
In the present invention, prepare graphite oxide initially with two benches low temperature process, concentrated sulphuric acid is added in graphite, first warp
Cross-20 DEG C ~-10 DEG C low temperature to stir 5-12 hour, then after 0 DEG C ~ 5 DEG C stirrings 5-12 hour, add potassium permanganate solution system
Standby graphite oxide, uses two benches low temperature process, and concentrated sulphuric acid carries out pre-oxidation to graphite, adds potassium permanganate and carries out graphite
In profound oxidizing process, the degree of oxidation of graphite oxide can be significantly improved, prepare high intensity MC Buddhist nun in follow-up preparation one
In dragon composite junction brick, improve graphene oxide dispersibility in MC nylon.
Using CTAB to be modified graphite oxide processing, modified graphite oxide specific surface area is big, with matrix Buddhist nun simultaneously
Dragon has and contacts more fully；The most modified graphite oxide and TDI are easy to react, and result is divided at modified graphite oxide
Son introduces NCO.These characteristics strengthen the strong interaction between modified graphene oxide and nylon molecules, carry
Both interface adhesions high.
Using modified graphene oxide to be modified MC nylon processing, the one prepared prepares high intensity MC nylon
Composite junction brick possesses excellent combination property, on the basis of keeping the original hot strength of MC nylon and hardness, uses asphaltic base
The mechanical property of fibre reinforced material can be adsorbed and the harmful gas of removing in tail gas and dust material greatly, joins
Close and use plasticizer, age resistor, self-control modified hydrotalcite, attapulgite clay, nano titanium oxide, nano-cerium oxide, promotion
Agent etc. are adjuvant, and component raw material prepares reasonable science, and the composition of interpolation not only can have the effective material ensureing its protection to be difficult to
Burning, and the too high burning of temperature also will not produce harmful gas；Wherein, self-control modified hydrotalcite is by a certain amount of
Magnesium aluminum-hydrotalcite be scattered in the deionized water of de-CO2 makes serosity after the NaH2PO4 2H2O of excess is dissolved in water is joined
Becoming solution to be poured slowly in serosity, heated and stirred also regulates PH to about 3.7 with acetic acid, reacts 3 hours, treat under reflux temperature
After natural cooling, with deionized water wash product the filtration of de-CO2 until filtrate PH=7, then it is dried and prepares, with at present
The brucite used on market, has the most high temperature resistant, fire prevention, fire-retardant advantage.
Detailed description of the invention
For being fully understood by the purpose of the present invention, feature and effect, by following specific embodiment, the present invention is done in detail
Describe in detail bright.
Embodiment one:
Under cryosel is bathed, adding 30ml concentrated sulphuric acid in the there-necked flask equipped with 1g graphite (325 mesh), mixture stirs at-15 DEG C
After mixing 12 hours certain times of reaction, then 0 DEG C of stirring reaction 5 hours, it is then slowly added into 2g potassium permanganate, is warming up to 35
DEG C, after reaction certain time, add deionized water, then be warming up to 90 DEG C, be eventually adding H2O2Become golden yellow to product, obtain
Graphite oxide solution, adds 0.2gCTAB in product, and graphite oxide settles the most rapidly, filters, washs, 50
DEG C vacuum drying 24 hours, i.e. obtains the modified graphene oxide modified with CTAB.
Embodiment 2
Under cryosel is bathed, adding 30ml concentrated sulphuric acid in the there-necked flask equipped with 1g graphite (325 mesh), mixture stirs at-10 DEG C
After mixing 10 hours certain times of reaction, then 0 DEG C of stirring reaction 3 hours, it is then slowly added into 2.3g potassium permanganate, is warming up to
35 DEG C, after reaction certain time, add deionized water, then be warming up to 90 DEG C, be eventually adding H2O2Become golden yellow to product,
To graphite oxide solution, adding 0.3gCTAB in product, graphite oxide settles the most rapidly, filters, washs,
50 DEG C are vacuum dried 24 hours, i.e. obtain the modified graphene oxide modified with CTAB.
Embodiment 3
Under cryosel is bathed, adding 30ml concentrated sulphuric acid in the there-necked flask equipped with 1g graphite (325 mesh), mixture stirs at-20 DEG C
After mixing 12 hours certain times of reaction, then 0 DEG C of stirring reaction 6 hours, it is then slowly added into 3g potassium permanganate, is warming up to 35
DEG C, after reaction certain time, add deionized water, then be warming up to 90 DEG C, be eventually adding H2O2Become golden yellow to product, obtain
Graphite oxide solution, adds 0.1gCTAB in product, and graphite oxide settles the most rapidly, filters, washs, 50
DEG C vacuum drying 24 hours, i.e. obtains the modified graphene oxide modified with CTAB.
B. the graphite oxide of high oxidation degree is prepared；
B. the graphite oxide using cetyl trimethylammonium bromide to obtain step a is modified processing, and to changing of obtaining
Property graphite oxide use and ultrasonic obtain graphene oxide；
C. situ aggregation method is used to prepare MC nylon/modified graphene oxide nano composite material；
D. add non-halogenated organophosphinate, hexamethylenetetramine, tri-methyl-amyl triethoxysilane, conductive mica powder,
Conductive nano graphite powder, the trimer of polyisocyanates, polytetrafluoroethylene fibre, nanoparticle active agent, plasticizer, age resistor, from
Modified hydrotalcite processed, attapulgite clay, nano titanium oxide, nano-cerium oxide, accelerator；
E. after remaining component being pulverized and mixed, standby after crossing 100-200 mesh screen；Stir prepared high temperature 90-100 DEG C
Base material；
F. by compound, base material being extruded into adobe by vacuum extruder, the vacuum of vacuum extruder is 1.0-1.8Mpa,
Extrusion pressure is 15-20Mpa；
Each component proportion described is: graphene oxide 5-10 weight portion, non-halogenated organophosphinate 5-7 part, six methines
Tetramine 8-10 part, tri-methyl-amyl triethoxysilane 2-4 part, conductive mica powder 0.3-0.5 weight portion, conductive nano graphite powder
0.2-0.4 weight portion, the trimer 0.8-1 weight portion of polyisocyanates, polytetrafluoroethylene fibre 1-2 weight portion, nano active
Agent 20-30 weight portion, plasticizer 2-8 weight portion, age resistor 1-5 weight portion, self-control modified hydrotalcite 2-6 weight portion, attapulgite
Stone clay 10-18 weight portion, nano titanium oxide 8-12 weight portion, nano-cerium oxide 6-14 weight portion, accelerator 2-6 weight
Part；
G. by after the adobe of step (f) under field conditions (factors) dry in the sun 15 days at a temperature of 700 DEG C sinter molding；Base material is put into
In Mechanical processing of casting machine, first adding pressurizing melting on vulcanizing press at foundry goods, melt temperature is 160-190 DEG C, after constant temperature 3-5h certainly
So cooling.
Described nanoparticle active agent is the compositions of MgO, Al2O3, Si3N4, BN；
The preparation method of described self-control modified hydrotalcite is: a certain amount of magnesium aluminum-hydrotalcite is scattered in the deionized water of de-CO2
In make serosity after the NaH2PO4 2H2O of excess is dissolved in water institute wiring solution-forming is poured slowly in serosity, heated and stirred is also used
Acetic acid regulation PH to about 3.7, reacts 3 hours under reflux temperature, after natural cooling, with the deionized water wash of de-CO2
Product also filters until filtrate PH=7, is then dried to obtain self-control modified hydrotalcite.
In the present invention, prepared the graphite oxide of high oxidation degree by low temperature two-phase method, and use CTAB that it is carried out
Modification, on the one hand improves graphene oxide dispersibility in MC nylon matrix, and on the other hand, graphene oxide is at Hou Chu
There is finishing time during reason long, the problem that technique is loaded down with trivial details, this also constrains graphene oxide and realizes application, uses
CTAB is added directly in graphite oxide solution, and while modification, graphite oxide solution has been carried out at flocculation by CTAB
Reason, is substantially shorter the last handling process of graphite oxide, improves graphite oxide preparation efficiency, therefore, uses CTAB to oxidation stone
Ink carries out post processing, shortens graphite oxide aftertreatment technology while modification.Use modified graphene oxide to MC Buddhist nun
Dragon is modified, and in the case of modified graphene oxide content is little, one prepares high intensity MC nylon composite junction brick with regard to energy
Reach good mechanical property.
Above example is the preferred embodiments of the present invention, and those skilled in the art draw according to technical scheme
Rational technique scheme is also within scope.
Claims (6)
1. the preparation method of a high intensity MC nylon modified fibre composite base material, it is characterised in that comprise the following steps:
The graphite oxide of preparation high oxidation degree；
B. the graphite oxide using cetyl trimethylammonium bromide to obtain step a is modified processing, and to changing of obtaining
Property graphite oxide use and ultrasonic obtain graphene oxide；
C. situ aggregation method is used to prepare MC nylon/modified graphene oxide nano composite material；
D. add non-halogenated organophosphinate, hexamethylenetetramine, tri-methyl-amyl triethoxysilane, conductive mica powder,
Conductive nano graphite powder, the trimer of polyisocyanates, polytetrafluoroethylene fibre, nanoparticle active agent, plasticizer, age resistor, from
Modified hydrotalcite processed, attapulgite clay, nano titanium oxide, nano-cerium oxide, accelerator；
E. after remaining component being pulverized and mixed, standby after crossing 100-200 mesh screen；Stir prepared high temperature 90-100 DEG C
Base material；
F. by compound, base material being extruded into adobe by vacuum extruder, the vacuum of vacuum extruder is 1.0-1.8Mpa,
Extrusion pressure is 15-20Mpa；
Each component proportion described is: graphene oxide 5-10 weight portion, non-halogenated organophosphinate 5-7 part, six methines
Tetramine 8-10 part, tri-methyl-amyl triethoxysilane 2-4 part, conductive mica powder 0.3-0.5 weight portion, conductive nano graphite powder
0.2-0.4 weight portion, the trimer 0.8-1 weight portion of polyisocyanates, polytetrafluoroethylene fibre 1-2 weight portion, nano active
Agent 20-30 weight portion, plasticizer 2-8 weight portion, age resistor 1-5 weight portion, self-control modified hydrotalcite 2-6 weight portion, attapulgite
Stone clay 10-18 weight portion, nano titanium oxide 8-12 weight portion, nano-cerium oxide 6-14 weight portion, accelerator 2-6 weight
Part；
G. by after the adobe of step (f) under field conditions (factors) dry in the sun 15 days at a temperature of 700 DEG C sinter molding；Base material is put into
In Mechanical processing of casting machine, first adding pressurizing melting on vulcanizing press at foundry goods, melt temperature is 160-190 DEG C, after constant temperature 3-5h certainly
So cooling.
A kind of preparation method preparing high intensity MC nylon composite junction brick, it is characterised in that: step
Rapid a prepares high oxidation degree graphite oxide include: added by concentrated sulphuric acid in graphite, through-20 DEG C ~-10 DEG C low temperature stirring 5-
12 hours, then after 0 DEG C ~ 5 DEG C stirrings 5-12 hour, addition potassium permanganate carries out oxidation reaction and obtains graphite oxide solution.
A kind of preparation method preparing high intensity MC nylon composite junction brick, it is characterised in that: step
Rapid b use cetyl trimethylammonium bromide (CTAB) to include graphene oxide modification: aoxidized in step a
Graphite solution is directly added into CTAB, CTAB graphite oxide is flocculated and modified-reaction obtains modified graphite oxide solution.
4. a kind of preparation method preparing high intensity MC nylon composite junction brick as described in claim 2-3, it is characterised in that
Graphite with the mass ratio of CTAB is: 10:1 ~ 20:1, and graphite with the mass ratio of potassium permanganate is: 1:1 ~ 1:5.
A kind of preparation method preparing high intensity MC nylon composite junction brick, it is characterised in that: step
In rapid c, use situ aggregation method to prepare MC nylon/modified graphene oxide nano composite material and include: caprolactam is heated
To 70 DEG C-100 DEG C to melted, the modified graphene oxide solution that mass fraction is 0.05% ~ 5% is joined caprolactam and melts
Adding a certain amount of catalyst in liquid, decompression distillation removes by-product in 30-60 minute, is eventually adding a certain amount of activator, fast
Speed is poured into after stirring in preheated mould, reacts 1-4 hour at 80-150 DEG C.
A kind of preparation method preparing high intensity MC nylon composite junction brick, it is characterised in that institute
Stating catalyst is sodium hydroxide, and described activator is 2,4 toluene diisocyanate (TDI).
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| CN108912304A (en) * | 2018-07-25 | 2018-11-30 | 福州大学 | A kind of preparation method of high-termal conductivity modified TPU film |
| CN109468702A (en) * | 2018-10-17 | 2019-03-15 | 浙江方圆聚合纤有限公司 | A kind of preparation method of 6 fiber of graphene modified nylon |
| CN113683773A (en) * | 2021-07-29 | 2021-11-23 | 扬州尼尔工程塑料有限公司 | Method for synergistically enhancing MC nylon composite material by using nano particles |
| CN113864424A (en) * | 2021-09-28 | 2021-12-31 | 重庆市大足区宝丽得物资有限公司 | MC nylon wheel and production method thereof |
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| CN108912304A (en) * | 2018-07-25 | 2018-11-30 | 福州大学 | A kind of preparation method of high-termal conductivity modified TPU film |
| CN109468702A (en) * | 2018-10-17 | 2019-03-15 | 浙江方圆聚合纤有限公司 | A kind of preparation method of 6 fiber of graphene modified nylon |
| CN113683773A (en) * | 2021-07-29 | 2021-11-23 | 扬州尼尔工程塑料有限公司 | Method for synergistically enhancing MC nylon composite material by using nano particles |
| CN113864424A (en) * | 2021-09-28 | 2021-12-31 | 重庆市大足区宝丽得物资有限公司 | MC nylon wheel and production method thereof |
| CN113864424B (en) * | 2021-09-28 | 2023-09-15 | 重庆市大足区宝丽得物资有限公司 | MC nylon wheel and production method thereof |
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Application publication date: 20161207 |