CN108047701A - A kind of corrosion-resistant polyamide and preparation method thereof - Google Patents
A kind of corrosion-resistant polyamide and preparation method thereof Download PDFInfo
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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
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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K2003/3045—Sulfates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention discloses a kind of corrosion-resistant polyamides, belong to resin making technique field, the corrosion-resistant polyamide, including following raw material：Polyamide, ABS resin, polyflon, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin, dimethicone, makrolon, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate, zinc stearate, diatomite, silane coupling agent KH 560, corrosion-resistant modified additive, the corrosion-resistant polyamide is by preparing base-material, prepare modified materials, and by base-material, the materials such as modified materials mixing and etc. made of.The polyamide that the present invention is prepared has excellent corrosion resistance.
Description
Technical field
The present invention relates to the technical field of resin preparation process more particularly to a kind of corrosion-resistant polyamide and its preparations
Method.
Background technology
Polyamide is the condensation polymer type high-molecular compound for having in molecule-CONH structures, it usually by binary acid and
Diamine is obtained through polycondensation.The advantages of polyamide is most prominent is especially narrow for the scope of softening point, and not as other thermoplasticity
Resin is such, and there are one the processes for gradually curing or softening, and just cause when temperature is slightly less than fusing point and hastily cure.Polyamide
Resin has preferable resistance to chemical reagents, can resist soda acid and vegetable oil, mineral oil etc..Due in its molecule have amino, carbonyl,
Amide groups isopolarity base, therefore for the modelings such as timber, pottery, paper, cloth, brass, aluminium and phenolic resin, polyester resin, polyethylene
Material all has good glue performance.
A kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：CN105885036A)”
A kind of polyamide and preparation method thereof is disclosed, main chain contains propane diamine unit and oxalic acid unit, wherein, propane diamine list
Member is from the mixture of 1,2- propane diamine, 1,3-PD or both, the preparation method of the polyamide, including as follows
Step：In the presence of the solvent or it is solvent-free in the case of, by diamine monomer system and oxalate diester monomer containing propylene glycol
Mixing in room temperature to prepolymerization is carried out at a temperature of 150 DEG C, obtains prepolymer, and the prepolymer of gained is carried out melt polymerization or solid
Phase-polymerization, obtains polyamide, does not change polyamide high temperature resistant, low water suction, and monomer used is easy to get extensively, and price is low
It is honest and clean.But its corrosion resistance the needs of can not meeting in actual use.
The content of the invention
To solve technical problem present in background technology, the present invention proposes a kind of corrosion-resistant polyamide and its preparation
Method, to solve in a kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：
CN105885036A the problem of polyamide corrosion resistance is insufficient disclosed in) ".
A kind of corrosion-resistant polyamide proposed by the present invention, including following raw material：Polyamide, ABS resin, poly- four
Fluoroethylene resin, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin, dimethyl-silicon
Oil, makrolon, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide,
Polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate, zinc stearate, diatomite, silane coupling agent KH-560, corrosion-resistant modification help
Agent；
The zinc stearate, diatomite, silane coupling agent KH-560, the weight ratio of corrosion-resistant modified additive are (4-6)：
(6-9)：(1-3)：(14-18).
Further, the zinc stearate, diatomite, silane coupling agent KH-560, the weight ratio of corrosion-resistant modified additive
For 5：7.5：2：16.
Further, in units of parts by weight, including following raw material：80-120 parts of polyamide, ABS resin 35-45
Part, 15-25 parts of polyflon, 5-15 parts of epoxy acrylic resin, 4-8 parts of propoxylated bisphenol, butadiene rubber 3-9
It is part, 2-6 parts of organic siliconresin, 1-5 parts of alkyd resin, 2-5 parts of dimethicone, 1-5 parts of makrolon, 3-9 parts of polylactic acid, different
4-8 parts of cyanate, 2-6 parts of methyl ethyl ketone peroxide, 1-5 parts of chlorinated paraffin, 1-5 parts of polyether acrylate, nano-aluminum hydroxide 3-6
Part, 1-5 parts of polyphosphoric acids aluminium, 2-6 parts of hydroxyethyl cellulose, 1-5 parts of zinc borate, 4-6 parts of zinc stearate, 6-9 parts of diatomite, silicon
It is 1-3 parts of alkane coupling agent KH-560, modified additive 14-18 parts corrosion-resistant.
Further, the raw material of the corrosion-resistant modified additive includes by weight：40-50 parts of methyl methacrylate,
4-8 parts of neopelex, 4-9 parts of alkylphenol polyoxyethylene ether, 3-6 parts of ammonium persulfate, -174 4-8 of silane coupling A
Part, 2-5 parts of isopropyl titanate, 3-6 parts of montmorillonite powder, 1-5 parts of barium sulfate, 3-6 parts of weathered coal, 2-5 parts of seawood meal, bentonite 1-
5 parts, 3-6 parts of zeolite powder, 4-9 parts of nano-titanium dioxide.
Further, the corrosion-resistant modified additive is prepared by following technique：Methyl methacrylate is subtracted
Pressure distillation, then adds in neopelex and alkylphenol polyoxyethylene ether is uniformly mixed, and 20-40min is stirred by ultrasonic, so
After be warming up to 65-85 DEG C, then add in ammonium persulfate and silane coupling A -174, stir 5-15min, it is different then to add metatitanic acid
Propyl ester is uniformly mixed, and is then adjusted pH to 7-8 with ammonium hydroxide, is cooled to room temperature, is filtered under diminished pressure and takes filter cake, by will be in after Washing of Filter Cake
45-55 DEG C of dry 22-26h, grinding obtain material a；Then montmorillonite powder, barium sulfate, weathered coal, seaweed are added in into material a
Powder, bentonite, zeolite powder and nano-titanium dioxide are uniformly mixed, and ultrasound-mechanical agitation disperses 2-4h in 45-55 DEG C of water-bath,
Stratification removes supernatant liquor, lower reaction product layer is filtered, and washs, 750-850 DEG C is dried under vacuum to constant weight, grinds
Mill crosses 150-250 mesh sieves to get to corrosion-resistant modified additive.
The present invention also provides a kind of preparation methods of corrosion-resistant polyamide, include the following steps：
S1, by polyamide, ABS resin, polyflon, epoxy acrylic resin, propoxylated bisphenol,
Butadiene rubber, organic siliconresin, alkyd resin are uniformly mixed, and are stirred 10-30min in 850-1050r/min rotating speeds, are warming up to
80-90 DEG C, 20-40min is kept the temperature, then adds in dimethicone, makrolon, polylactic acid, isocyanates, peroxidating first and second
Ketone, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed,
Ball milling postcooling to room temperature obtains base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 60-80 DEG C, keep the temperature 10-
Then 20min adds in silane coupling agent KH-560 and is uniformly mixed, is continuously heating to 110-120 DEG C, keeps the temperature 5-15min, be cooled to
Room temperature obtains modified materials；
S3, base-material is warming up to 90-110 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 80-
90 DEG C, 20-30min is kept the temperature, then 1-2h is stirred in 1350-1550r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide
Resin.
The invention has the advantages that：
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that corrosion resistant using the corrosion-resistant polyamides of embodiment 1-3
Corrosion can significantly improve；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that zinc stearate, diatomite, silane coupling agent KH-560, resistance to
Corrosion modified additive adds simultaneously plays synergistic effect in corrosion-resistant polyamide is prepared, and significantly improves corrosion-resistant poly-
The corrosion resistance of amide resin, this may be：Zinc stearate, diatomite, silane coupling agent KH-560, corrosion-resistant modified additive
It is applied to as modified system in the preparation of polyamide, the graft modification of silane coupling agent KH-560 make use of to act on, it is real
The base-material for having showed zinc stearate, the hydroxyl of diatomite and corrosion-resistant modified additive surface and polyamide realizes grafting, assigns
The excellent corrosion resistance of polyamide, while make use of the corrosion-resistant humidification of corrosion-resistant modified additive, wherein resistance to
Corrode modified additive by the way that methyl methacrylate is evaporated under reduced pressure, then add in neopelex and alkyl phenol
Polyoxyethylene ether is uniformly mixed, and then ultrasonic agitation heats up, then add in ammonium persulfate and silane coupling A -174, stirs,
Then addition isopropyl titanate is uniformly mixed, and is then adjusted pH with ammonium hydroxide, is cooled to room temperature, is filtered under diminished pressure and takes filter cake, by filter cake
Dry after washing, grinding obtains material a；Then montmorillonite powder, barium sulfate, weathered coal, seawood meal, swelling are added in into material a
Soil, zeolite powder and nano-titanium dioxide are uniformly mixed, and ultrasound-mechanical agitation is disperseed in water-bath, stratification, and removal upper strata is clear
Liquid filters lower reaction product layer, and washing is dried under vacuum to constant weight, grinds, and sieves to get to corrosion-resistant modified additive,
It applies in the preparation of polyamide of the present invention, under the action of silane coupling agent KH-560, realizes and polyamide
Major ingredient carry out grafting combination, effectively increase the corrosion resistance of polyamide.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
Bright rather than for limiting the invention, any modification made on the basis of the present invention, equivalent substitution etc. are in this hair
In bright protection domain.
In embodiment, the corrosion-resistant polyamide, in units of parts by weight, including following raw material：Polyamide resin
80-120 parts of fat, 35-45 parts of ABS resin, 15-25 parts of polyflon, 5-15 parts of epoxy acrylic resin, propoxylation
4-8 parts of bisphenol-A, 3-9 parts of butadiene rubber, 2-6 parts of organic siliconresin, 1-5 parts of alkyd resin, 2-5 parts of dimethicone, poly- carbon
1-5 parts of acid esters, 3-9 parts of polylactic acid, 4-8 parts of isocyanates, 2-6 parts of methyl ethyl ketone peroxide, 1-5 parts of chlorinated paraffin, polyethers propylene
It is 1-5 parts of acid esters, 3-6 parts of nano-aluminum hydroxide, 1-5 parts of polyphosphoric acids aluminium, 2-6 parts of hydroxyethyl cellulose, 1-5 parts of zinc borate, hard
It is 4-6 parts of resin acid zinc, 6-9 parts of diatomite, 1-3 parts of silane coupling agent KH-560, modified additive 14-18 parts corrosion-resistant.
The corrosion-resistant modified additive is prepared by following technique：By weight by 40-50 parts of methyl methacrylates
It is evaporated under reduced pressure, then adds in 4-8 parts of neopelexes and 4-9 parts of alkylphenol polyoxyethylene ether are uniformly mixed, surpassed
Sound stirs 20-40min, then heats to 65-85 DEG C, then adds in 3-6 parts of ammonium persulfates and 4-8 parts of silane coupling A -174,
5-15min is stirred, 2-5 parts of isopropyl titanates is then added and is uniformly mixed, then adjust pH to 7-8 with ammonium hydroxide, be cooled to room temperature,
It is filtered under diminished pressure and takes filter cake, will will be ground in 45-55 DEG C of dry 22-26h and obtain material a after Washing of Filter Cake；Then into material a
Add in 3-6 parts of montmorillonite powders, 1-5 parts of barium sulfate, 3-6 parts of weathered coals, 2-5 portions of seawood meals, 1-5 parts of bentonites, 3-6 parts of zeolite powders
It is uniformly mixed with 4-9 parts of nano-titanium dioxides, ultrasound-mechanical agitation disperses 2-4h in 45-55 DEG C of water-bath, and stratification is gone
Except supernatant liquor, lower reaction product layer is filtered, is washed, 750-850 DEG C is dried under vacuum to constant weight, and 150-250 is crossed in grinding
Mesh sieve is to get to corrosion-resistant modified additive.
The preparation method of the corrosion-resistant polyamide, comprises the following steps：S1, by polyamide, ABS resin,
Polyflon, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin mixing
Uniformly, 10-30min is stirred in 850-1050r/min rotating speeds, is warming up to 80-90 DEG C, kept the temperature 20-40min, then add in diformazan
Base silicone oil, makrolon, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nanometer hydroxide
Aluminium, polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 60-80 DEG C, keep the temperature 10-
Then 20min adds in silane coupling agent KH-560 and is uniformly mixed, is continuously heating to 110-120 DEG C, keeps the temperature 5-15min, be cooled to
Room temperature obtains modified materials；
S3, base-material is warming up to 90-110 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 80-
90 DEG C, 20-30min is kept the temperature, then 1-2h is stirred in 1350-1550r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide
Resin.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of corrosion-resistant polyamide, in units of parts by weight, including following raw material：100 parts of polyamide, ABS
40 parts of resin, 20 parts of polyflon, 10 parts of epoxy acrylic resin, 6 parts of propoxylated bisphenol, 6 parts of butadiene rubber,
4 parts of organic siliconresin, 3 parts of alkyd resin, 3.5 parts of dimethicone, 3 parts of makrolon, 6 parts of polylactic acid, 6 parts of isocyanates,
4 parts of methyl ethyl ketone peroxide, 3 parts of chlorinated paraffin, 3 parts of polyether acrylate, 4.5 parts of nano-aluminum hydroxide, 3 parts of polyphosphoric acids aluminium,
It is 4 parts of hydroxyethyl cellulose, 3 parts of zinc borate, 5 parts of zinc stearate, 7.5 parts of diatomite, 2 parts of silane coupling agent KH-560, corrosion-resistant
16 parts of modified additive.
The corrosion-resistant modified additive is prepared by following technique：45 parts of methyl methacrylates are carried out by weight
Then vacuum distillation adds in 6 parts of neopelexes and 7 parts of alkylphenol polyoxyethylene ether is uniformly mixed, be stirred by ultrasonic
30min then heats to 75 DEG C, then adds in 4.5 parts of ammonium persulfates and 6 parts of silane coupling A -174, stirs 10min, then
3.5 parts of isopropyl titanates of addition are uniformly mixed, and are then adjusted pH to 7.5 with ammonium hydroxide, are cooled to room temperature, are filtered under diminished pressure and take filter cake,
It will will be ground in 50 DEG C of dryings for 24 hours and obtain material a after Washing of Filter Cake；Then into material a add in 4.5 parts of montmorillonite powders, 3 parts
Barium sulfate, 4.5 parts of weathered coals, 3.5 portions of seawood meals, 3 parts of bentonites, 4.5 parts of zeolite powders and 7 parts of nano-titanium dioxide mixing are equal
Even, ultrasound-mechanical agitation disperses 3h in 50 DEG C of water-baths, and stratification removes supernatant liquor, lower reaction product layer is taken out
Filter, washing, 800 DEG C are dried under vacuum to constant weight, grinding, cross 200 mesh sieves to get to corrosion-resistant modified additive.
The preparation method of the corrosion-resistant polyamide, comprises the following steps：S1, by polyamide, ABS resin,
Polyflon, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin mixing
Uniformly, 20min is stirred in 950r/min rotating speeds, is warming up to 85 DEG C, keep the temperature 30min, then add in dimethicone, poly- carbonic acid
Ester, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids
Aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 70 DEG C, keep the temperature 15min, then
It adds in silane coupling agent KH-560 to be uniformly mixed, is continuously heating to 115 DEG C, keep the temperature 10min, be cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 100 DEG C, keeps the temperature 25min, be subsequently added into modified materials and be uniformly mixed, be cooled to 85 DEG C, heat preservation
25min then stirs 1.5h in 1450r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide.
Embodiment 2
A kind of corrosion-resistant polyamide, in units of parts by weight, including following raw material：80 parts of polyamide, ABS trees
45 parts of fat, 15 parts of polyflon, 4 parts of propoxylated bisphenol, 9 parts of butadiene rubber, have 15 parts of epoxy acrylic resin
2 parts of machine silicones, 5 parts of alkyd resin, 2 parts of dimethicone, 5 parts of makrolon, 3 parts of polylactic acid, 8 parts of isocyanates, peroxide
Change 2 parts of methyl ethyl ketone, 5 parts of chlorinated paraffin, 1 part of polyether acrylate, 6 parts of nano-aluminum hydroxide, 1 part of polyphosphoric acids aluminium, ethoxy
6 parts of cellulose, 1 part of zinc borate, 6 parts of zinc stearate, 6 parts of diatomite, 3 parts of silane coupling agent KH-560, corrosion-resistant modified additive
14 parts.
The corrosion-resistant modified additive is prepared by following technique：40 parts of methyl methacrylates are carried out by weight
Then vacuum distillation adds in 8 parts of neopelexes and 4 parts of alkylphenol polyoxyethylene ether is uniformly mixed, be stirred by ultrasonic
40min then heats to 65 DEG C, then adds in 6 parts of ammonium persulfates and 4 parts of silane coupling A -174, stirs 15min, Ran Houtian
2 parts of isopropyl titanates is added to be uniformly mixed, then pH to 8 is adjusted with ammonium hydroxide, is cooled to room temperature, is filtered under diminished pressure and takes filter cake, by filter cake
It will be ground in 45 DEG C of dry 26h and obtain material a after washing；Then 3 parts of montmorillonite powders, 5 parts of barium sulfate, 3 are added in into material a
Part weathered coal, 5 portions of seawood meals, 1 part of bentonite, 6 parts of zeolite powders and 4 parts of nano-titanium dioxides are uniformly mixed, in 55 DEG C of water-baths
Ultrasound-mechanical agitation disperses 2h, and stratification removes supernatant liquor, lower reaction product layer is filtered, and washs, and 850 DEG C true
Sky is dry to constant weight, grinding, crosses 150 mesh sieves to get to corrosion-resistant modified additive.
The preparation method of the corrosion-resistant polyamide, comprises the following steps：S1, by polyamide, ABS resin,
Polyflon, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin mixing
Uniformly, 30min is stirred in 850r/min rotating speeds, is warming up to 80 DEG C, keep the temperature 40min, then add in dimethicone, poly- carbonic acid
Ester, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids
Aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 60 DEG C, keep the temperature 20min, then
It adds in silane coupling agent KH-560 to be uniformly mixed, is continuously heating to 110 DEG C, keep the temperature 15min, be cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 90 DEG C, keeps the temperature 35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 80 DEG C, heat preservation
30min then stirs 2h in 1350r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide.
Embodiment 3
A kind of corrosion-resistant polyamide, in units of parts by weight, including following raw material：120 parts of polyamide, ABS
35 parts of resin, 25 parts of polyflon, 5 parts of epoxy acrylic resin, 8 parts of propoxylated bisphenol, 3 parts of butadiene rubber,
6 parts of organic siliconresin, 1 part of alkyd resin, 5 parts of dimethicone, 1 part of makrolon, 9 parts of polylactic acid, 4 parts of isocyanates, mistake
6 parts of Methyl Ethyl Ketone Oxidation, 1 part of chlorinated paraffin, 5 parts of polyether acrylate, 3 parts of nano-aluminum hydroxide, 5 parts of polyphosphoric acids aluminium, hydroxyl second
2 parts of base cellulose, 5 parts of zinc borate, 4 parts of zinc stearate, 9 parts of diatomite, 1 part of silane coupling agent KH-560, corrosion-resistant modification help
18 parts of agent.
The corrosion-resistant modified additive is prepared by following technique：50 parts of methyl methacrylates are carried out by weight
Then vacuum distillation adds in 4 parts of neopelexes and 9 parts of alkylphenol polyoxyethylene ether is uniformly mixed, be stirred by ultrasonic
20min then heats to 85 DEG C, then adds in 3 parts of ammonium persulfates and 8 parts of silane coupling A -174, stirs 5min, Ran Houtian
5 parts of isopropyl titanates is added to be uniformly mixed, then pH to 7 is adjusted with ammonium hydroxide, is cooled to room temperature, is filtered under diminished pressure and takes filter cake, by filter cake
It will be ground in 55 DEG C of dry 22h and obtain material a after washing；Then 6 parts of montmorillonite powders, 1 part of barium sulfate, 6 are added in into material a
Part weathered coal, 2 portions of seawood meals, 5 parts of bentonites, 3 parts of zeolite powders and 9 parts of nano-titanium dioxides are uniformly mixed, in 45 DEG C of water-baths
Ultrasound-mechanical agitation disperses 4h, and stratification removes supernatant liquor, lower reaction product layer is filtered, and washs, and 750 DEG C true
Sky is dry to constant weight, grinding, crosses 250 mesh sieves to get to corrosion-resistant modified additive.
The preparation method of the corrosion-resistant polyamide, comprises the following steps：S1, by polyamide, ABS resin,
Polyflon, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin mixing
Uniformly, 10min is stirred in 1050r/min rotating speeds, is warming up to 90 DEG C, keep the temperature 20min, then add in dimethicone, poly- carbonic acid
Ester, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids
Aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 80 DEG C, keep the temperature 10min, then
It adds in silane coupling agent KH-560 to be uniformly mixed, is continuously heating to 120 DEG C, keep the temperature 5min, be cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 110 DEG C, keeps the temperature 15min, be subsequently added into modified materials and be uniformly mixed, be cooled to 90 DEG C, heat preservation
20min then stirs 1h in 1550r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw material of corrosion-resistant polyamide
Lack zinc stearate, diatomite, silane coupling agent KH-560, corrosion-resistant modified additive.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw material of corrosion-resistant polyamide
Lack zinc stearate.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw material of corrosion-resistant polyamide
Lack diatomite.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw material of corrosion-resistant polyamide
Lack silane coupling agent KH-560.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw material of corrosion-resistant polyamide
Lack corrosion-resistant modified additive.
Comparative example 6
Using a kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：
CN105885036A) " technique of embodiment 1 prepares polyamide.
The polyamide for measuring embodiment 1-3 and comparative example 1-6 carries out indices detection, and obtained testing result is such as
Following table：
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that corrosion resistant using the corrosion-resistant polyamides of embodiment 1-3
Corrosion can significantly improve；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that zinc stearate, diatomite, silane coupling agent KH-560, resistance to
Corrosion modified additive adds simultaneously plays synergistic effect in corrosion-resistant polyamide is prepared, and significantly improves corrosion-resistant poly-
The corrosion resistance of amide resin, this may be：Zinc stearate, diatomite, silane coupling agent KH-560, corrosion-resistant modified additive
It is applied to as modified system in the preparation of polyamide, the graft modification of silane coupling agent KH-560 make use of to act on, it is real
The base-material for having showed zinc stearate, the hydroxyl of diatomite and corrosion-resistant modified additive surface and polyamide realizes grafting, assigns
The excellent corrosion resistance of polyamide, while make use of the corrosion-resistant humidification of corrosion-resistant modified additive, wherein resistance to
Corrode modified additive by the way that methyl methacrylate is evaporated under reduced pressure, then add in neopelex and alkyl phenol
Polyoxyethylene ether is uniformly mixed, and then ultrasonic agitation heats up, then add in ammonium persulfate and silane coupling A -174, stirs,
Then addition isopropyl titanate is uniformly mixed, and is then adjusted pH with ammonium hydroxide, is cooled to room temperature, is filtered under diminished pressure and takes filter cake, by filter cake
Dry after washing, grinding obtains material a；Then montmorillonite powder, barium sulfate, weathered coal, seawood meal, swelling are added in into material a
Soil, zeolite powder and nano-titanium dioxide are uniformly mixed, and ultrasound-mechanical agitation is disperseed in water-bath, stratification, and removal upper strata is clear
Liquid filters lower reaction product layer, and washing is dried under vacuum to constant weight, grinds, and sieves to get to corrosion-resistant modified additive,
It applies in the preparation of polyamide of the present invention, under the action of silane coupling agent KH-560, realizes and polyamide
Major ingredient carry out grafting combination, effectively increase the corrosion resistance of polyamide.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of corrosion-resistant polyamide, which is characterized in that including following raw material：Polyamide, ABS resin, polytetrafluoro
Vinyl, epoxy acrylic resin, propoxylated bisphenol, butadiene rubber, organic siliconresin, alkyd resin, dimethyl-silicon
Oil, makrolon, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorinated paraffin, polyether acrylate, nano-aluminum hydroxide,
Polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate, zinc stearate, diatomite, silane coupling agent KH-560, corrosion-resistant modification help
Agent；
The zinc stearate, diatomite, silane coupling agent KH-560, the weight ratio of corrosion-resistant modified additive are (4-6)：(6-9)：
(1-3)：(14-18).
2. corrosion-resistant polyamide according to claim 1, which is characterized in that the zinc stearate, diatomite, silane
Coupling agent KH-560, the weight ratio of corrosion-resistant modified additive are 5：7.5：2：16.
3. corrosion-resistant polyamide according to claim 1 or 2, which is characterized in that in units of parts by weight, including with
Lower raw material：80-120 parts of polyamide, 35-45 parts of ABS resin, 15-25 parts of polyflon, epoxy acrylic resin
5-15 parts, 4-8 parts of propoxylated bisphenol, 3-9 parts of butadiene rubber, 2-6 parts of organic siliconresin, 1-5 parts of alkyd resin, dimethyl
2-5 parts of silicone oil, 1-5 parts of makrolon, 3-9 parts of polylactic acid, 4-8 parts of isocyanates, 2-6 parts of methyl ethyl ketone peroxide, chlorinated paraffin
1-5 parts, 1-5 parts of polyether acrylate, 3-6 parts of nano-aluminum hydroxide, 1-5 parts of polyphosphoric acids aluminium, 2-6 parts of hydroxyethyl cellulose,
1-5 parts of zinc borate, 4-6 parts of zinc stearate, 6-9 parts of diatomite, 1-3 parts of silane coupling agent KH-560, corrosion-resistant modified additive
14-18 parts.
4. according to the corrosion-resistant polyamide of claim 1-3 any one of them, which is characterized in that the corrosion-resistant modification helps
The raw material of agent includes by weight：40-50 parts of methyl methacrylate, 4-8 parts of neopelex, alkyl phenol polyoxy second
4-9 parts of alkene ether, 3-6 parts of ammonium persulfate, -1744-8 parts of silane coupling A, 2-5 parts of isopropyl titanate, 3-6 parts of montmorillonite powder, sulphur
Sour barium 1-5 parts, 3-6 parts of weathered coal, 2-5 parts of seawood meal, 1-5 parts of bentonite, 3-6 parts of zeolite powder, 4-9 parts of nano-titanium dioxide.
5. according to the corrosion-resistant polyamide of claim 1-4 any one of them, which is characterized in that the corrosion-resistant modification helps
Agent is prepared by following technique：Methyl methacrylate is evaporated under reduced pressure, then add in neopelex and
Alkylphenol polyoxyethylene ether is uniformly mixed, and 20-40min is stirred by ultrasonic, then heats to 65-85 DEG C, then adds in ammonium persulfate
With silane coupling A -174,5-15min is stirred, isopropyl titanate is then added and is uniformly mixed, then adjust pH to 7- with ammonium hydroxide
8, it is cooled to room temperature, is filtered under diminished pressure and takes filter cake, will will be ground in 45-55 DEG C of dry 22-26h and obtain material a after Washing of Filter Cake；
Then montmorillonite powder, barium sulfate, weathered coal, seawood meal, bentonite, zeolite powder and nano-titanium dioxide is added in into material a to mix
It closes uniformly, ultrasound-mechanical agitation disperses 2-4h in 45-55 DEG C of water-bath, and stratification removes supernatant liquor, lower floor is reacted
Product is filtered, and washing, 750-850 DEG C is dried under vacuum to constant weight, grinding, crosses 150-250 mesh sieves to get to corrosion-resistant modification
Auxiliary agent.
A kind of 6. preparation method according to the corrosion-resistant polyamide of claim 1-5 any one of them, which is characterized in that bag
Include following steps：
S1, by polyamide, ABS resin, polyflon, epoxy acrylic resin, propoxylated bisphenol, along fourth
Rubber, organic siliconresin, alkyd resin are uniformly mixed, and are stirred 10-30min in 850-1050r/min rotating speeds, are warming up to 80-90
DEG C, 20-40min is kept the temperature, then adds in dimethicone, makrolon, polylactic acid, isocyanates, methyl ethyl ketone peroxide, chlorination
Paraffin, polyether acrylate, nano-aluminum hydroxide, polyphosphoric acids aluminium, hydroxyethyl cellulose, zinc borate are uniformly mixed, after ball milling
It is cooled to room temperature to obtain base-material；
S2, zinc stearate, diatomite, corrosion-resistant modified additive are uniformly mixed, are warming up to 60-80 DEG C, keep the temperature 10-20min, so
Silane coupling agent KH-560 is added in afterwards to be uniformly mixed, and is continuously heating to 110-120 DEG C, is kept the temperature 5-15min, be cooled to room temperature to obtain
Modified materials；
S3, base-material is warming up to 90-110 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 80-90
DEG C, 20-30min is kept the temperature, then 1-2h is stirred in 1350-1550r/min rotating speeds, is cooled to room temperature to obtain corrosion-resistant polyamide resin
Fat.
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| CN111690320A (en) * | 2020-06-24 | 2020-09-22 | 赣县洪顺工艺厂 | High-adhesion toy coating resin and preparation method thereof |
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| US20170099739A1 (en) * | 2014-03-07 | 2017-04-06 | Azotek Co., Ltd. | Method of manufacturing metal substrate |
| CN106674866A (en) * | 2016-12-12 | 2017-05-17 | 天长市康宁塑胶科技有限公司 | High-hardness corrosion-resistant modified plastic material |
| CN107163492A (en) * | 2017-06-19 | 2017-09-15 | 合肥斯科尔智能科技有限公司 | A kind of auto manufacturing high-temperature resistant anti-corrosive 3D printing material and preparation method thereof |
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| US20170099739A1 (en) * | 2014-03-07 | 2017-04-06 | Azotek Co., Ltd. | Method of manufacturing metal substrate |
| CN106674866A (en) * | 2016-12-12 | 2017-05-17 | 天长市康宁塑胶科技有限公司 | High-hardness corrosion-resistant modified plastic material |
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Application publication date: 20180518 |