CN109135266A - A kind of processing method of plastics high stability antistatic agent - Google Patents
A kind of processing method of plastics high stability antistatic agent Download PDFInfo
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- CN109135266A CN109135266A CN201811074427.0A CN201811074427A CN109135266A CN 109135266 A CN109135266 A CN 109135266A CN 201811074427 A CN201811074427 A CN 201811074427A CN 109135266 A CN109135266 A CN 109135266A
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- reaction kettle
- antistatic agent
- high stability
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- 239000004033 plastic Substances 0.000 title claims abstract description 37
- 229920003023 plastic Polymers 0.000 title claims abstract description 37
- 239000002216 antistatic agent Substances 0.000 title claims abstract description 35
- 238000003672 processing method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 30
- 230000002708 enhancing effect Effects 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 20
- 239000011265 semifinished product Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims description 69
- 238000012545 processing Methods 0.000 claims description 34
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000010445 mica Substances 0.000 claims description 29
- 229910052618 mica group Inorganic materials 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000001354 calcination Methods 0.000 claims description 16
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 239000004793 Polystyrene Substances 0.000 claims description 12
- 229920002223 polystyrene Polymers 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 230000005611 electricity Effects 0.000 claims description 10
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 10
- 150000002910 rare earth metals Chemical class 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 150000003233 pyrroles Chemical class 0.000 claims description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 3
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 15
- 239000004615 ingredient Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 229920006146 polyetheresteramide block copolymer Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000000052 vinegar Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- -1 graphite alkene Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- PBCKVROHSSNSDY-UHFFFAOYSA-N 2-methylprop-2-enoic acid;sodium Chemical compound [Na].CC(=C)C(O)=O PBCKVROHSSNSDY-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005367 electrostatic precipitation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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 discloses a kind of plastics processing methods of high stability antistatic agent, include the following steps: (1) anti-electricity enhancing material preparation, the preparation of (2) semi-finished product, the preparation of (3) finished product.The present invention provides a kind of preparation methods of antistatic agent, its simple process, each step collocation is reasonable, it is easy to promote and utilize, antistatic agent obtained can significantly reduce the resistance value of plastics, promote its antistatic effect, additionally it is possible to improve whole mechanics and use quality, and stability is high, the great market competitiveness and production and application value.
Description
Technical field
The invention belongs to plastic processing processing technology fields, and in particular to a kind of plastics high stability antistatic agent adds
Work method.
Background technique
Most of high molecular materials accumulation easy to produce static electricity in production and use, so that electrostatic precipitation, electrostatic be caused to put
The bad phenomenons such as electricity.It can produce spark when serious, cause fire or explosion, make troubles to industrial production and daily life.
Currently, plastic product is widely used in people's lives, and common frosting resistance is all larger than 1012Ω or more,
Electric conductivity is very poor, easy to produce static electricity during packed and transported and be not easy to guide, and very big harm is caused to product.It is quiet with resisting
The increasingly extensive application of electric agent also proposed increasingly higher demands to the performance of antistatic agent.
Plastics are the widely used high molecular synthetic materials of modern society, it have very high surface resistivity (25 DEG C,
RH60%, resistivity 1017Ω).Thus, once be charged by friction, electrostatic not easily passs through conductive remove and is trapped in frosting.
Due to the presence of electrostatic, not only influence the beauty (dust suction etc.) of plastic products, more important is the manufacture for influencing plastic products and
It uses.Plastics package antistatic agent reduces Polymer Surface resistivity and charge density for plastic products face, to reach solution
Destatic the purpose of harm.
Traditional antistatic agent is made of the surfactant of small molecule, it contains hydrophilic radical and lipophilic group.By
It is not exclusively compatible in it and resin itself, therefore antistatic agent can be from resin internal migration to resin surface.It is traditional antistatic
Agent needs can act below certain damp condition, and hydrophilic radical can promote frosting to be readily wetted by water, to dredge
Electrostatic charge reduces the surface resistivity of plastics.Only can just it work after conventional antistatic agents molecular migration is to surface, plastics
Internal antistatic agent molecule moves about to surface, until completely consume, thus its function and effect is only in certain time model
It encloses interior effective.
Macromolecule permanent antistatic agent can only be added in base-material by the method for mixing.It is not by migrating to modeling
Expect surface, and be positioned against plastics inner and form the Percolation Network with conductive capability, takes off surface and sheet as access
Intracorporal electrostatic charge reduces resistivity.Compared with conventional antistatic agents, antistatic effect is lasting, no induction period, is not wiped
It is influenced with conditions such as washings；Because its electric conductivity reaches not by water layer, thus relies on the relative humidity of air
Property is small, and the mechanical performance and heat resistance of product are unaffected.
CN102051156A discloses a kind of poly-vinegar ethers Polymer-metallic Catalyst, mainly by the original of following parts by weight
Material prepares: 100 parts of poly glycol monomethyl ether metering system vinegar, 30-250 parts of methyl methacrylate vinegar, methacrylic acid
Sodium or methacrylic acid with sodium carbonate mixture 2-50 parts, 1-30 parts and AIBNO.1-5 parts of sodium metasilicate.The invention does not use
Unstable and toxic sodium perchlorate keeps production process more environmentally-friendly, and furthermore the invention also improves the temperature-resistance characteristic of product,
Use scope is expanded, can be applied in the materials such as PET, PA, PB, PE, PP, PS, ABS, PVC, PLA of antistatic.But this is anti-
Electrostatic agent is as most existing usual products, and there is influence the qualities such as plastic product mechanics.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of processing side of plastics high stability antistatic agent is provided
Method.
The present invention is achieved by the following technical solutions:
A kind of plastics processing method of high stability antistatic agent, includes the following steps:
(1) anti-electricity enhancing material preparation:
A. mica powder is put into and carries out ball-milling treatment in ball mill, took out after 2500 meshes after the completion particulate mica powder is standby
With；
B. it the resulting particulate mica powder of a will be operated being put into calcining furnace and carry out calcination processing, the temperature for controlling calcining is 740 ~
It 760 DEG C, is taken out after 1 ~ 1.5h spare；
C. by polystyrene and operation b, treated that particulate mica powder is put into incinerator jointly, keeps oxygen in incinerator
Abundance, is heated to 1000 ~ 1100 DEG C, taken out after full combustion mixture A is spare；
D. pyrroles and ethanol water are carried out mixing according to volume ratio 1:90 ~ 95 to put into reaction kettle, then will operates c system
The mixture A obtained is put into reaction kettle, while reaction kettle being placed under condition of ice bath, is stirred with 400 ~ 450 revs/min of revolving speed
30 ~ 35min of processing is mixed, then to ammonium persulfate solution is added in reaction kettle, is filtered after 10 ~ 12h of reaction treatment, Zhi Houyong
After ethyl alcohol, deionized water alternate repetition clean 5 ~ 7 times, it is finally putting into and takes out anti-after being dried 4 ~ 5h in vacuum oven
Electricity enhancing material is spare；
(2) prepared by semi-finished product:
A. caprolactam, binary acid, deionized water are corresponded to mix according to 95 ~ 100:14 of weight ratio ~ 18:2 ~ 4 and is put into
In reaction kettle, it is then passed through argon gas into reaction kettle, keeping the pressure in reaction kettle is 0.5 ~ 0.55MPa, while by reaction kettle
Interior temperature heating remains 270 ~ 280 DEG C, be stirred continuously after 2 ~ 3h of processing mixture B is spare；
B. the polyethers of mixture B gross mass 70 ~ 75%, 0.5 ~ 1% rare earth nitric acid are added into operation a treated reaction kettle
Anti- electricity enhancing material made from the step of salt, 8 ~ 10% (1), is passed through argon gas into reaction kettle again, and the pressure in holding reaction kettle is
0.4 ~ 0.5MPa, while the temperature heating in reaction kettle is remained 290 ~ 300 DEG C, after being stirred continuously 3 ~ 4h of processing, it will react
Kettle is unloaded to normal temperature and pressure, finally takes out to obtain semi-finished product for standby；
(3) prepared by finished product:
Step (2) resulting semi-finished product are put into after 3 ~ 5h of drying in oven processing to take out and are got product.
Further, polystyrene described in step (1) operation c and the corresponding throwing of operation b treated particulate mica powder
The weight ratio entered is 3:2.
Further, the volume fraction of ethyl alcohol is 50 ~ 55% in ethanol water described in step (1) operation d；It is described
Operation c made from mixture A input amount be ethanol water gross mass 4 ~ 5%.
Further, the additional amount of ammonium persulfate solution described in step (1) operation d is ethanol water total volume
33 ~ 35%, the mass fraction of ammonium persulfate solution is 0.7 ~ 0.9%；The temperature in vacuum oven is controlled when the drying process
It is 68 ~ 73 DEG C.
Further, speed of agitator when stir process described in step (2) operation a is 300 ~ 400 revs/min.
Further, it is any in cerous nitrate, lanthanum nitrate, yttrium nitrate that step (2), which operates rare earth nitrades described in b,
It is a kind of.
Further, speed of agitator when stir process described in step (2) operation b is 500 ~ 600 revs/min.
Further, it is 90 ~ 95 DEG C that the temperature in baking oven is controlled when drying and processing described in step (3).
The present invention has carried out special Optimal improvements to the preparation method of antistatic agent, enhances its antistatic property, and
And the drawbacks of optimizing its binding ability between high molecule plastic, improving use, improve the quality used.Wherein first make
For a kind of anti-electricity enhancing material ingredient, calcination processing first is carried out to mica powder, improves its specific surface area and adsorption reaction ability,
Then it is mixed to be placed in incinerator jointly with polystyrene and carry out burning processing, under conditions of high temperature, oxygen are sufficient, gathered
Styrene is sufficiently burned as carbon source, cooperate particulate mica powder catalytic action, form a large amount of nanoscale graphite alkene at
Point, in the environment of adequate heat, nanoscale graphite alkene is inserted and fixed in the ectonexine of particulate mica powder, is formd one kind and is received
The mixture A ingredient that the insertion of meter level graphene combines, has then carried out semi-finished product preparation, has been prepared for a kind of polyetheresteramide block
Copolymer, this copolymer have the function of improvement plastics electrical property, will be special in polymerization in order to further enhance its using effect
The anti-electricity enhancing material of system is added polymerization, and the entirety that this anti-electricity enhancing material can cooperate ester bond to enhance this block copolymer is resistance to
The qualities such as temperature, intensity, and help form the high conductive network of increasingly complex conduction efficiency, further improve antistatic energy
Power；And after the anti-electricity enhancing material of composite crosslinking, then make an addition in plastics, the mechanical quality for improving plastics can be optimized, improve biography
The problem of antistatic agent damage plastics mechanical property of uniting；Finally by the polyether ester amides of this anti-electricity enhancing material addition and subsequent preparation
Compounding, improves the antistatic using effect of polyether ester amides.
The present invention has the advantage that compared with prior art
The present invention provides a kind of preparation method of antistatic agent, simple process, each step collocation rationally, is answered convenient for promoting
With antistatic agent obtained can significantly reduce the resistance value of plastics, promote its antistatic effect, additionally it is possible to improve whole
Mechanics uses quality, and stability is high, the great market competitiveness and production and application value.
Specific embodiment
Embodiment 1
A kind of plastics processing method of high stability antistatic agent, includes the following steps:
(1) anti-electricity enhancing material preparation:
A. mica powder is put into and carries out ball-milling treatment in ball mill, took out after 2500 meshes after the completion particulate mica powder is standby
With；
B. it the resulting particulate mica powder of a will be operated is put into calcining furnace and carry out calcination processing, the temperature for controlling calcining is 740
DEG C, it is taken out after 1h spare；
C. by polystyrene and operation b, treated that particulate mica powder is put into incinerator jointly, keeps oxygen in incinerator
Abundance, is heated to 1000 DEG C, taken out after full combustion mixture A is spare；
D. pyrroles and ethanol water are carried out mixing according to volume ratio 1:90 to put into reaction kettle, then operation c is made
Mixture A put into reaction kettle, while reaction kettle being placed under condition of ice bath, with 400 revs/min of revolving speed stir process
30min is filtered after reaction treatment 10h then to ammonium persulfate solution is added in reaction kettle, uses ethyl alcohol, deionization later
Water alternate repetition clean 5 times after, be finally putting into vacuum oven be dried 4h after take out it is anti-electricity enhancing material it is spare；
(2) prepared by semi-finished product:
A. caprolactam, binary acid, deionized water are corresponded to mix according to weight ratio 95:14:2 and are put into reaction kettle,
Then argon gas is passed through into reaction kettle, keeping the pressure in reaction kettle is 0.5MPa, while the temperature in reaction kettle being heated and is protected
Holding is 270 DEG C, be stirred continuously processing 2h after mixture B it is spare；
B. 70% polyethers of mixture B gross mass, 0.5% rare earth nitrades, 8% are added into operation a treated reaction kettle
Anti- electricity enhancing material, is passed through argon gas into reaction kettle again made from step (1), and keeping the pressure in reaction kettle is 0.4MPa, together
When the temperature heating in reaction kettle remained 290 DEG C, after being stirred continuously processing 3h, reaction kettle is unloaded to normal temperature and pressure, finally
Take out to obtain semi-finished product for standby；
(3) prepared by finished product:
Step (2) resulting semi-finished product are put into after drying in oven processing 3h to take out and are got product.
Further, polystyrene described in step (1) operation c and the corresponding throwing of operation b treated particulate mica powder
The weight ratio entered is 3:2.
Further, the volume fraction of ethyl alcohol is 50% in ethanol water described in step (1) operation d；The behaviour
The input amount for making mixture A made from c is the 4% of ethanol water gross mass.
Further, the additional amount of ammonium persulfate solution described in step (1) operation d is ethanol water total volume
33%, the mass fraction of ammonium persulfate solution is 0.7%；It is 68 DEG C that the temperature in vacuum oven is controlled when the drying process.
Further, speed of agitator when stir process described in step (2) operation a is 300 revs/min.
Further, rare earth nitrades described in step (2) operation b are cerous nitrate.
Further, speed of agitator when stir process described in step (2) operation b is 500 revs/min.
Further, it is 90 DEG C that the temperature in baking oven is controlled when drying and processing described in step (3).
Embodiment 2
A kind of plastics processing method of high stability antistatic agent, includes the following steps:
(1) anti-electricity enhancing material preparation:
A. mica powder is put into and carries out ball-milling treatment in ball mill, took out after 2500 meshes after the completion particulate mica powder is standby
With；
B. it the resulting particulate mica powder of a will be operated is put into calcining furnace and carry out calcination processing, the temperature for controlling calcining is 750
DEG C, it is taken out after 1.3h spare；
C. by polystyrene and operation b, treated that particulate mica powder is put into incinerator jointly, keeps oxygen in incinerator
Abundance, is heated to 1050 DEG C, taken out after full combustion mixture A is spare；
D. pyrroles and ethanol water are carried out mixing according to volume ratio 1:93 to put into reaction kettle, then operation c is made
Mixture A put into reaction kettle, while reaction kettle being placed under condition of ice bath, with 430 revs/min of revolving speed stir process
32min is filtered after reaction treatment 11h then to ammonium persulfate solution is added in reaction kettle, uses ethyl alcohol, deionization later
Water alternate repetition clean 6 times after, be finally putting into vacuum oven be dried 4.5h after take out it is anti-electricity enhancing material it is spare；
(2) prepared by semi-finished product:
A. caprolactam, binary acid, deionized water are corresponded to mix according to weight ratio 98:16:3 and are put into reaction kettle,
Then argon gas is passed through into reaction kettle, keeping the pressure in reaction kettle is 0.53MPa, while the temperature in reaction kettle being heated and is protected
Holding is 275 DEG C, be stirred continuously processing 2.5h after mixture B it is spare；
B. 73% polyethers of mixture B gross mass, 0.8% rare earth nitrades, 9% are added into operation a treated reaction kettle
Anti- electricity enhancing material, is passed through argon gas into reaction kettle again made from step (1), and keeping the pressure in reaction kettle is 0.45MPa, together
When the temperature heating in reaction kettle remained 295 DEG C, after being stirred continuously processing 3.6h, reaction kettle is unloaded to normal temperature and pressure, most
After take out to obtain semi-finished product for standby；
(3) prepared by finished product:
Step (2) resulting semi-finished product are put into after drying in oven processing 4h to take out and are got product.
Further, polystyrene described in step (1) operation c and the corresponding throwing of operation b treated particulate mica powder
The weight ratio entered is 3:2.
Further, the volume fraction of ethyl alcohol is 53% in ethanol water described in step (1) operation d；The behaviour
The input amount for making mixture A made from c is the 4.5% of ethanol water gross mass.
Further, the additional amount of ammonium persulfate solution described in step (1) operation d is ethanol water total volume
34%, the mass fraction of ammonium persulfate solution is 0.8%；It is 70 DEG C that the temperature in vacuum oven is controlled when the drying process.
Further, speed of agitator when stir process described in step (2) operation a is 350 revs/min.
Further, rare earth nitrades described in step (2) operation b are lanthanum nitrate.
Further, speed of agitator when stir process described in step (2) operation b is 550 revs/min.
Further, it is 93 DEG C that the temperature in baking oven is controlled when drying and processing described in step (3).
Embodiment 3
A kind of plastics processing method of high stability antistatic agent, includes the following steps:
(1) anti-electricity enhancing material preparation:
A. mica powder is put into and carries out ball-milling treatment in ball mill, took out after 2500 meshes after the completion particulate mica powder is standby
With；
B. it the resulting particulate mica powder of a will be operated is put into calcining furnace and carry out calcination processing, the temperature for controlling calcining is 760
DEG C, it is taken out after 1.5h spare；
C. by polystyrene and operation b, treated that particulate mica powder is put into incinerator jointly, keeps oxygen in incinerator
Abundance, is heated to 1100 DEG C, taken out after full combustion mixture A is spare；
D. pyrroles and ethanol water are carried out mixing according to volume ratio 1:95 to put into reaction kettle, then operation c is made
Mixture A put into reaction kettle, while reaction kettle being placed under condition of ice bath, with 450 revs/min of revolving speed stir process
35min is filtered after reaction treatment 12h then to ammonium persulfate solution is added in reaction kettle, uses ethyl alcohol, deionization later
Water alternate repetition clean 7 times after, be finally putting into vacuum oven be dried 5h after take out it is anti-electricity enhancing material it is spare；
(2) prepared by semi-finished product:
A. caprolactam, binary acid, deionized water are corresponded to mix according to weight ratio 100:18:4 and are put into reaction kettle,
Then argon gas is passed through into reaction kettle, keeping the pressure in reaction kettle is 0.55MPa, while the temperature in reaction kettle being heated and is protected
Holding is 280 DEG C, be stirred continuously processing 3h after mixture B it is spare；
B. 75% polyethers of mixture B gross mass, 1% rare earth nitrades, 10% are added into operation a treated reaction kettle
Anti- electricity enhancing material, is passed through argon gas into reaction kettle again made from step (1), and keeping the pressure in reaction kettle is 0.5MPa, together
When the temperature heating in reaction kettle remained 300 DEG C, after being stirred continuously processing 4h, reaction kettle is unloaded to normal temperature and pressure, finally
Take out to obtain semi-finished product for standby；
(3) prepared by finished product:
Step (2) resulting semi-finished product are put into after drying in oven processing 5h to take out and are got product.
Further, polystyrene described in step (1) operation c and the corresponding throwing of operation b treated particulate mica powder
The weight ratio entered is 3:2.
Further, the volume fraction of ethyl alcohol is 55% in ethanol water described in step (1) operation d；The behaviour
The input amount for making mixture A made from c is the 5% of ethanol water gross mass.
Further, the additional amount of ammonium persulfate solution described in step (1) operation d is ethanol water total volume
35%, the mass fraction of ammonium persulfate solution is 0.9%；It is 73 DEG C that the temperature in vacuum oven is controlled when the drying process.
Further, speed of agitator when stir process described in step (2) operation a is 400 revs/min.
Further, rare earth nitrades described in step (2) operation b are yttrium nitrate.
Further, speed of agitator when stir process described in step (2) operation b is 600 revs/min.
Further, it is 95 DEG C that the temperature in baking oven is controlled when drying and processing described in step (3).
Comparative example 1
This comparative example 1 compared with Example 2, in the anti-electricity enhancing material preparation of step (1), eliminates the processing of operation c, removes
Furthermore method and step is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, in the anti-electricity enhancing material preparation of step (1), eliminates the processing of operation d, removes
Furthermore method and step is all the same.
Comparative example 3
This comparative example 3 compared with Example 2, step (2) semi-finished product preparation in, with etc. mass parts mica powder replace step
Suddenly anti-electricity enhancing material ingredient, method and step in addition to this made from (1) are all the same.
Comparative example 4
This comparative example 4 compared with Example 2, step (2) semi-finished product preparation in, with etc. mass parts graphene replace step
Suddenly anti-electricity enhancing material ingredient, method and step in addition to this made from (1) are all the same.
Comparative example 5
This comparative example 5 compared with Example 2, in the preparation of step (2) semi-finished product, eliminates anti-electricity made from step (1)
Enhancing material ingredient, method and step in addition to this are all the same.
Control group
Application No. is: a kind of high temperature resistance polyester ether Polymer Antistatic Agent disclosed in 201010179071.4.
In order to compare effect of the present invention, by above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
The corresponding antistatic agent obtained of comparative example 4, comparative example 5, control group is for adding in the addition preparation of ABS plastic
Weight percent be 5%, be processed into plastic sample according to same process, performance detection then carried out to sample, it is specific to compare
Data are as shown in table 1 below:
Table 1
Note: surface resistivity described in upper table 1 is tested referring to the standard of ASTM D257, and the temperature of experiment is 25 DEG C, phase
To humidity RH60%；The tensile strength is tested referring to GB/T 1040；The Izod notched impact strength reference
GB/T 1843 is tested.
The synthesis service performance for the antistatic agent that the method for the present invention is processed into it can be seen from upper table 1 is good, can be apparent
Promote the antistatic property of plastics, and stay in grade, the great market competitiveness.
Claims (8)
1. a kind of plastics processing method of high stability antistatic agent, which comprises the steps of:
(1) anti-electricity enhancing material preparation:
A. mica powder is put into and carries out ball-milling treatment in ball mill, took out after 2500 meshes after the completion particulate mica powder is standby
With；
B. it the resulting particulate mica powder of a will be operated being put into calcining furnace and carry out calcination processing, the temperature for controlling calcining is 740 ~
It 760 DEG C, is taken out after 1 ~ 1.5h spare；
C. by polystyrene and operation b, treated that particulate mica powder is put into incinerator jointly, keeps oxygen in incinerator
Abundance, is heated to 1000 ~ 1100 DEG C, taken out after full combustion mixture A is spare；
D. pyrroles and ethanol water are carried out mixing according to volume ratio 1:90 ~ 95 to put into reaction kettle, then will operates c system
The mixture A obtained is put into reaction kettle, while reaction kettle being placed under condition of ice bath, is stirred with 400 ~ 450 revs/min of revolving speed
30 ~ 35min of processing is mixed, then to ammonium persulfate solution is added in reaction kettle, is filtered after 10 ~ 12h of reaction treatment, Zhi Houyong
After ethyl alcohol, deionized water alternate repetition clean 5 ~ 7 times, it is finally putting into and takes out anti-after being dried 4 ~ 5h in vacuum oven
Electricity enhancing material is spare；
(2) prepared by semi-finished product:
A. caprolactam, binary acid, deionized water are corresponded to mix according to 95 ~ 100:14 of weight ratio ~ 18:2 ~ 4 and is put into
In reaction kettle, it is then passed through argon gas into reaction kettle, keeping the pressure in reaction kettle is 0.5 ~ 0.55MPa, while by reaction kettle
Interior temperature heating remains 270 ~ 280 DEG C, be stirred continuously after 2 ~ 3h of processing mixture B is spare；
B. the polyethers of mixture B gross mass 70 ~ 75%, 0.5 ~ 1% rare earth nitric acid are added into operation a treated reaction kettle
Anti- electricity enhancing material made from the step of salt, 8 ~ 10% (1), is passed through argon gas into reaction kettle again, and the pressure in holding reaction kettle is
0.4 ~ 0.5MPa, while the temperature heating in reaction kettle is remained 290 ~ 300 DEG C, after being stirred continuously 3 ~ 4h of processing, it will react
Kettle is unloaded to normal temperature and pressure, finally takes out to obtain semi-finished product for standby；
(3) prepared by finished product:
Step (2) resulting semi-finished product are put into after 3 ~ 5h of drying in oven processing to take out and are got product.
2. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(1) weight ratio for operating polystyrene described in c and the corresponding investment of operation b treated particulate mica powder is 3:2.
3. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(1) volume fraction for operating ethyl alcohol in ethanol water described in d is 50 ~ 55%；Mixture A's made from the operation c
Input amount is the 4 ~ 5% of ethanol water gross mass.
4. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(1) additional amount for operating ammonium persulfate solution described in d is the 33 ~ 35% of ethanol water total volume, ammonium persulfate solution
Mass fraction is 0.7 ~ 0.9%；It is 68 ~ 73 DEG C that the temperature in vacuum oven is controlled when the drying process.
5. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(2) speed of agitator when operating stir process described in a is 300 ~ 400 revs/min.
6. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(2) rare earth nitrades described in b are operated as any one in cerous nitrate, lanthanum nitrate, yttrium nitrate.
7. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(2) speed of agitator when operating stir process described in b is 500 ~ 600 revs/min.
8. a kind of processing method of plastics high stability antistatic agent according to claim 1, which is characterized in that step
(3) temperature when drying and processing described in control baking oven is 90 ~ 95 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231883A (en) * | 2018-09-19 | 2019-01-18 | 蚌埠星烁新材料科技有限公司 | A kind of weather-resistant and high-strength degree lacquer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398100A (en) * | 2016-09-30 | 2017-02-15 | 美的集团股份有限公司 | Anti-static and easy-to-clean material and preparation method thereof |
| CN106633778A (en) * | 2016-12-30 | 2017-05-10 | 东莞市奥能工程塑料有限公司 | High-content glass fiber reinforced antistatic PC composite material and preparation method thereof |
-
2018
- 2018-09-14 CN CN201811074427.0A patent/CN109135266A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398100A (en) * | 2016-09-30 | 2017-02-15 | 美的集团股份有限公司 | Anti-static and easy-to-clean material and preparation method thereof |
| CN106633778A (en) * | 2016-12-30 | 2017-05-10 | 东莞市奥能工程塑料有限公司 | High-content glass fiber reinforced antistatic PC composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231883A (en) * | 2018-09-19 | 2019-01-18 | 蚌埠星烁新材料科技有限公司 | A kind of weather-resistant and high-strength degree lacquer |
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