CN106380593A - Antibacterial MC (monomer casting) nylon composite material and preparation method thereof - Google Patents
Antibacterial MC (monomer casting) nylon composite material and preparation method thereof Download PDFInfo
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- CN106380593A CN106380593A CN201610848714.7A CN201610848714A CN106380593A CN 106380593 A CN106380593 A CN 106380593A CN 201610848714 A CN201610848714 A CN 201610848714A CN 106380593 A CN106380593 A CN 106380593A
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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
-
- 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
- C08K3/02—Elements
- C08K3/08—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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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)
Abstract
The invention relates to an antibacterial MC (monomer casting) nylon composite material and a preparation method thereof. The composite material comprises the following components in parts by weight: 100 parts of caprolactam, 0.1-10 parts of antibacterial modifier, 0.1-2 parts of catalyst, 0.1-2 parts of activator, 0.08-0.15 part of silane coupling agent and 3-6 parts of ethanol. The preparation method comprises the following steps: dissolving the silane coupling agent in the ethanol, adding the antibacterial modifier in batches, stirring, drying to obtain powder, adding the powder into the molten caprolactam, stirring, treating until no bubbles are generated, adding the catalyst, treating until no bubbles are generated, adding the activator, casting into a mold, keeping the temperature, cooling and demolding. The antibacterial modifier can not generate side effects on the anionic polymerization reaction of MC nylon, and has favorable compatibility with the polymer matrix. The obtained composite material can perform obvious antibacterial functions on the premise of keeping favorable inherent mechanical properties of the MC nylon.
Description
Technical field
The invention belongs to Polymer Synthesizing and manufacture field, particularly to a kind of antibacterial MC nylon composite materials and its preparation
Method.
Background technology
MC nylon, also known as nylon monomer-cast nylon, is to carry out anionic polymerisation by caprolactam monomer at ambient pressure, then warp
Cross a kind of engineering plastics with superior function of casting coagulation forming.MC nylon is as a kind of high engineering plastic of cost performance
Material, have that lightweight, intensity is high, self-lubricating, wear-resisting, anti-corrosion, insulation etc. multiple a little, have its application in every field.As
The module such as the modern packaging in food service industry and machine driving also has begun to be occurred using MC nylon " moulding Dai Gang ".In order to adapt to
Food service industry is inherently gradually increased for the demand of antibiotic plastic for the requirement of anti-microbial property aspect, market.
Content of the invention
The technical problem to be solved is to provide a kind of antibacterial MC nylon composite materials and preparation method thereof, passes through
Composite prepared by the method is to be integrally formed through a step to obtain, and need not be surface-treated again；Nano-antibacterial is modified
Agent can preferably be dispersed in MC nylon matrix after silane coupler process, it is to avoid occurs reuniting.Prepared is compound
Material, while remaining MC nylon premium properties, have also obtained the lifting of anti-microbial property aspect.
A kind of antibacterial MC nylon composite materials of the present invention, the component of described composite includes by weight：Acyl in oneself
100 parts of amine, antibacterial modified dose 0.1～10 part, 0.1～2 part of catalyst, 0.1～2 part of activator, silane coupler 0.08～
0.15 part.
The component of described composite includes by weight：100 parts of caprolactam, antibacterial modified dose 3 parts, catalyst
0.254 part, 0.362 part of activator, 0.10 part of silane coupler.
The component of described composite includes by weight：100 parts of caprolactam, antibacterial modified dose 5 parts, catalyst 0.5
Part, 0.412 part of activator, 0.15 part of silane coupler.
Described antibacterial modified dose is nano zine oxide, nano titanium oxide, nano silicon-based oxide, nanometer Ag and nanometer Cu
In at least one.
Described catalyst is metallic sodium, metallic potassium, NaOH, sodium caprolactam or caustic alcohol.
Described activator be toluene di-isocyanate(TDI), hexamethylene diisocyanate, methyl diphenylene diisocyanate, two
One of diphenylmethane diisocyanate.
Described silane coupler is one of KH550, KH560, KH570.
A kind of preparation method of the antibacterial MC nylon composite materials of the present invention, including：
(1) 0.08-0.15 part silane coupler is dissolved in 3-6 part ethanol, be dividedly in some parts antibacterial modified dose of 0.1-10 part, stir
Mix 30-60 minute, be dried, obtain powder, standby after cooling；Wherein, described number is weight portion；
(2) by after 100 parts of caprolactam meltings, add the powder in step (1), stirring, vacuumize dehydration to bubble-free
Produce, then release vacuum, add 0.1～2 part of catalyst, vacuumize, 110-140 DEG C of stirring (dehydration) produces to bubble-free,
Logical nitrogen protection releases vacuum, adds 0.1～2 part of activator, obtains treating aggressiveness system；Wherein, described number is weight portion；
(3) will aggressiveness system be treated to be cast in advance be preheated in 160～180 DEG C of mould in step (2), insulation 0.5～
1h, cooling, the demoulding, obtain antibacterial MC nylon composite materials.
It is to divide 2～3 times in described step (1) in batches；Be dried condition be：It is dried in 80-100 DEG C of vacuum drying chamber.
In described step (2), the method for caprolactam melting includes：Caprolactam is taken to be added in dry reactor, plus
Heat arrives 110-140 DEG C, makes caprolactam melted by heating.
In described step (2), the time of stirring (dehydration) is 20～30 minutes.
In the antibacterial MC nylon composite materials of the present invention antibacterial modified dose will not produce to MC nylon anionic polymerisation
Raw side effect, and can have good compatibility between fine dispersion, and polymeric matrix in polymerization system, this composite energy
While keeping MC nylon intrinsic good mechanical properties, play obvious antibacterial action.
Beneficial effect
Nanometer can be accomplished after silane coupler is processed in MC nylon matrix for antibacterial modified dose in material of the present invention
Level dispersion, and can be used as the degree of crystallinity crystallizing into epipole raising MC nylon.And then, MC nylon is keeping the same of its own mechanical performance
When, also can obtain certain anti-microbial property, be with a wide range of applications.
Brief description
Fig. 1 is the measured the anti-bacterial result schematic diagram (overlay film to nano zinc oxide modified MC nylon composite materials of embodiment 1
The bacterium colony flat board photo of gradient dilution coating after culture 24h wash-out)；Wherein, in figure C represents according to QB/T 2591-2003 test
Antibiotic plastic sample sets, 10-nThe multiple of culture is diluted, each little figure is the 3 of same dilution gradient after representing culture 24 hours
Individual parallel；
Fig. 2 is pure MC nylon the anti-bacterial result schematic diagram (the gradient dilution painting after overlay film culture 24h wash-out of reference examples 1 gained
The bacterium colony flat board photo of cloth)；Wherein, in figure B represent according to QB/T 2591-2003 test pure MC nylon samples group, 10-nTable
Dilute the multiple of culture after showing culture 24 hours, each little figure be 3 of same dilution gradient parallel.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) take 0.10 part of Silane coupling agent KH550,5 parts of ethanol, first KH550 is dissolved in ethanol, add to three times at twice
Enter 3 parts of nano zine oxide, stir 30 minutes, be then dried in 80 DEG C of vacuum drying chamber, obtain powder, standby after cooling；
(2) take 100 parts of caprolactams to be added in dry reactor, be heated to 110 DEG C, make caprolactam be subject to hot melt
Melt, after waiting it to melt completely, add above-mentioned powder modifier, obtain the mixed system containing modifying agent.
(3) mixed system containing modifying agent obtaining step (2) vacuumizes dehydration under agitation, until no longer
Bubble occurs, then releases vacuum；
(4) add 0.254 part of NaOH in the mixed system that step (3) obtains, vacuumize, temperature is maintained at 135
DEG C, it is dehydrated while stirring, continues 25 minutes, until no longer bubble, logical nitrogen protection releases vacuum；Add toluene diisocyanate
0.362 part of acid esters, obtains treating aggressiveness system；
(5) treat aggressiveness system to be cast in advance to be preheated in 180 DEG C of mould by what step (4) obtained, cold after insulation 0.5h
But to the room temperature demoulding, antibacterial MC nylon composite materials are obtained.
Above-mentioned number is weight portion.
Prepared MC nylon composite materials carry out anti-microbial property test according to QB T2591, as shown in figure 1, its antibiotic rate
For 99.3%, there is strong antibacterial action；Its coefficient of friction is 0.4128, and wear scar width is 5.13mm.
Embodiment 2
(1) take 0.15 part of silane coupler KH560,6 parts of ethanol, first KH560 is dissolved in ethanol, add to three times at twice
Enter 5 parts of nanometer Ag, stir 45 minutes, be then dried in 100 DEG C of vacuum drying chamber, obtain powder, standby after cooling；
(2) take 100 parts of caprolactams to be added in dry reactor, be heated to 135 DEG C, make caprolactam be subject to hot melt
Melt, after waiting it to melt completely, add above-mentioned powder modifier, obtain the mixed system containing modifying agent.
(3) mixed system containing modifying agent obtaining step (2) vacuumizes dehydration under agitation, until no longer
Bubble occurs, then releases vacuum；
(4) add 0.5 part of sodium caprolactam in the mixed system that step (3) obtains, vacuumize, temperature is maintained at 140
DEG C, it is dehydrated while stirring, continues 30 minutes, until no longer bubble, logical nitrogen protection releases vacuum；Add hexa-methylene two
0.412 part of isocyanates, obtains treating aggressiveness system；
(5) treat aggressiveness system to be cast in advance to be preheated in 160 DEG C of mould by what step (4) obtained, cold after insulation 0.8h
But to the room temperature demoulding, antibacterial MC nylon composite materials are obtained.
Above-mentioned number is weight portion.
Prepared MC nylon composite materials carry out anti-microbial property test according to QB T2591, and its antibiotic rate is 94.3%,
There is antibacterial action.
Reference examples 1
(1) caprolactam is added in dry reactor, is heated to 135 DEG C, makes caprolactam melted by heating；
(2) mixed system obtaining step (1) vacuumizes dehydration under agitation, until no longer bubble, so
Release vacuum afterwards；
(3) add 0.216 part of NaOH in the mixed system that step (2) obtains, vacuumize, temperature is maintained at 135
DEG C, it is dehydrated while stirring, continues 30 minutes, until no longer bubble, logical nitrogen protection releases vacuum；Add toluene diisocyanate
Acid esters, obtains treating aggressiveness system；
(4) treat aggressiveness system to be cast in advance to be preheated in 180 DEG C of mould by what step (3) obtained, cold after insulation 0.5h
But to room temperature, the demoulding.
Prepared MC nylon carries out anti-microbial property test according to QB T2591, as shown in Fig. 2 no anti-microbial property.
Claims (10)
1. a kind of antibacterial MC nylon composite materials are it is characterised in that the component of described composite includes by weight：Acyl in oneself
100 parts of amine, antibacterial modified dose 0.1～10 part, 0.1～2 part of catalyst, 0.1～2 part of activator, silane coupler 0.08～
0.15 part.
2. a kind of antibacterial MC nylon composite materials according to claim 1 are it is characterised in that the component of described composite
Include by weight：100 parts of caprolactam, antibacterial modified dose 3 parts, 0.254 part of catalyst, 0.362 part of activator, silane coupled
0.10 part of agent.
3. a kind of antibacterial MC nylon composite materials according to claim 1 are it is characterised in that the component of described composite
Include by weight：100 parts of caprolactam, antibacterial modified dose 5 parts, 0.5 part of catalyst, 0.412 part of activator, silane coupler
0.15 part.
4. a kind of antibacterial MC nylon composite materials according to claims 1 to 3 any one are it is characterised in that described resist
Bacterium modifying agent is at least one in nano zine oxide, nano titanium oxide, nano silicon-based oxide, nanometer Ag and nanometer Cu.
5. a kind of antibacterial MC nylon composite materials according to claims 1 to 3 any one are it is characterised in that described urge
Agent is metallic sodium, metallic potassium, NaOH, sodium caprolactam or caustic alcohol.
6. a kind of antibacterial MC nylon composite materials according to claims 1 to 3 any one are it is characterised in that described work
Agent is toluene di-isocyanate(TDI), hexamethylene diisocyanate, methyl diphenylene diisocyanate, dicyclohexyl methyl hydride two are different
One of cyanate.
7. a kind of antibacterial MC nylon composite materials according to claims 1 to 3 any one are it is characterised in that described silicon
Alkane coupling agent is one of KH550, KH560, KH570.
8. a kind of preparation method of antibacterial MC nylon composite materials, including：
(1) 0.08-0.15 part silane coupler is dissolved in 3-6 part ethanol, be dividedly in some parts antibacterial modified dose of 0.1-10 part, stirring
30-60 minute, is dried, obtains powder, standby after cooling；
(2) by after 100 parts of caprolactam meltings, add the powder in step (1), stirring, vacuumize dehydration and produce to bubble-free,
Then release vacuum, add 0.1～2 part of catalyst, vacuumize, 110-140 DEG C is stirred to bubble-free generation, is passed through protective atmosphere
Release vacuum, add 0.1～2 part of activator, obtain treating aggressiveness system；Wherein, above-mentioned number is weight portion；
(3) by treating in the mould that aggressiveness system is cast to 160～180 DEG C in step (2), it is incubated 0.5-1h, cooling, the demoulding, obtains
To antibacterial MC nylon composite materials.
9. a kind of preparation method of antibacterial MC nylon composite materials according to claim 8 is it is characterised in that described step
(1) it is to divide 2～3 times in batches；Be dried condition be：It is dried in 80-100 DEG C of vacuum drying chamber.
10. a kind of preparation method of antibacterial MC nylon composite materials according to claim 8 is it is characterised in that described step
Suddenly in (2), the time of 110-140 DEG C of stirring is 20～30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848714.7A CN106380593A (en) | 2016-09-23 | 2016-09-23 | Antibacterial MC (monomer casting) nylon composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848714.7A CN106380593A (en) | 2016-09-23 | 2016-09-23 | Antibacterial MC (monomer casting) nylon composite material and preparation method thereof |
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| CN201610848714.7A Pending CN106380593A (en) | 2016-09-23 | 2016-09-23 | Antibacterial MC (monomer casting) nylon composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114525616A (en) * | 2022-04-11 | 2022-05-24 | 吴江市兰天织造有限公司 | Double-thread nylon black silk double-layer down-filled cloth |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563192A (en) * | 2004-04-13 | 2005-01-12 | 上海宇航特种化学纤维厂 | Antibacterial polyamide and fiber, and preparation method |
| EP2093246A2 (en) * | 2008-02-20 | 2009-08-26 | Rhein Chemie Rheinau GmbH | Anionic polymerisation of lactams using special activators |
| CN102558846A (en) * | 2010-12-28 | 2012-07-11 | 合肥杰事杰新材料股份有限公司 | Nylon/titanium dioxide nanometer composite microsphere and preparation method thereof |
| CN103965465A (en) * | 2013-01-29 | 2014-08-06 | 合肥杰事杰新材料股份有限公司 | Casting nylon 6 nanometer composite material and preparation method thereof |
-
2016
- 2016-09-23 CN CN201610848714.7A patent/CN106380593A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563192A (en) * | 2004-04-13 | 2005-01-12 | 上海宇航特种化学纤维厂 | Antibacterial polyamide and fiber, and preparation method |
| EP2093246A2 (en) * | 2008-02-20 | 2009-08-26 | Rhein Chemie Rheinau GmbH | Anionic polymerisation of lactams using special activators |
| CN102558846A (en) * | 2010-12-28 | 2012-07-11 | 合肥杰事杰新材料股份有限公司 | Nylon/titanium dioxide nanometer composite microsphere and preparation method thereof |
| CN103965465A (en) * | 2013-01-29 | 2014-08-06 | 合肥杰事杰新材料股份有限公司 | Casting nylon 6 nanometer composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114525616A (en) * | 2022-04-11 | 2022-05-24 | 吴江市兰天织造有限公司 | Double-thread nylon black silk double-layer down-filled cloth |
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Application publication date: 20170208 |