CN110423401A - A kind of preparation method of polypropylene antioxidant - Google Patents
A kind of preparation method of polypropylene antioxidant Download PDFInfo
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- CN110423401A CN110423401A CN201910539892.5A CN201910539892A CN110423401A CN 110423401 A CN110423401 A CN 110423401A CN 201910539892 A CN201910539892 A CN 201910539892A CN 110423401 A CN110423401 A CN 110423401A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/36—Sulfonation; Sulfation
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/10—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to inorganic materials
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of the preparation methods of polypropylene antioxidant, belong to the technical field of antioxidant.The present invention is by sodium carbonate as raw material, it is mixed with auxiliary agent, by react with calcium chloride, pass through the effect of surfactant and ammonium hydrogen carbonate, form porous nanometer calcium carbonate, then mixed with mix monomer, form polymer engrafted nanometer calcium carbonate structure, and the effect for passing through activating agent, the polymer of formation is modified, form anion living polymerization object, finally again by being combined with extract, to form polypropylene antioxidant, it is poor that the present invention solves current polypropylene antioxidant thermostabilization, and the problem that compatibility is low.
Description
Technical field
The present invention relates to the technical fields of antioxidant, and in particular to a kind of preparation method of polypropylene antioxidant.
Background technique
Recently as the rapid growth of plastics production capacity, the productive consumption of antioxidant is also correspondinglyd increase.Plastics industry it is fast
Speed development, it is the development and application forward dedicateds of various new type functional plastic additives, multifunction, molecular weight, compound
The directions such as change, harmless to environment are developed.Plastics factors such as light, oxygen, heat in manufacture, processing, storage and use process act on,
It occur frequently that oxidative degradation, causes ageing of plastics, the intensity and appearance of plastics are influenced.As most common general-purpose plastics polypropylene
(PP) it is widely used to the packaging material of food, medical treatment, health product and cosmetics and other items.But because of conformation defect
And molecular structure is more sensitive to oxidation, it is easy to aging during processing use to make PP, and then reduce its service life.To make PP
Material is durable, needs to be added all kinds of anti-aging auxiliary agents into PP raw material, wherein the addition of antioxidant can delay PP material
Oxidative degradation.In order to extend the service life of plastics macromolecular material, inhibit or delay the oxidative degradation of polymer, it is usually used
Antioxidant.Antioxidant refers to that those can alleviate the substance of high molecular material Auto-oxidation reaction speed.The effect of antioxidant is to disappear
Except the free radical just generated, or promote the decomposition of hydroperoxides, prevents the progress of chain reaction.Antioxidant is by main and auxiliary
Two or more antioxidant compounds, and generates synergistic effect and plays superior performance.Free radical can be eliminated
Antioxidant have the compounds such as aromatic amine and hindered phenol and its derivative, referred to as primary antioxidant；Energy hydroperoxide decomposition resists
Oxygen agent has phosphorous and sulfur-bearing organic compound, referred to as auxiliary antioxidant.Hindered phenol is one of most effective antioxidant, structure
In contain-OH functional group, be easier to provide hydrogen atom, i.e., by proton donation, to destroy free radical autoxidation
Chain reaction.Currently, the antioxidant added in the plastic is broadly divided into three classes: Hinered phenols, hindered amines, Phosphorus and sulphur class are auxiliary
Aid anti-oxidants.Antioxidant 264 (2,6-di-tert-butyl p-cresol) is most widely used phenolic antioxidant, it belongs to single phenol type and is obstructed
Phenol antioxidant, 68-70 DEG C of fusing point；Because its production is easy, cheap, pollution-free, the market demand accounts for the half of phenolic antioxidant
More than.The shortcomings that antioxidant 264 is that protective benefits are less high, when processing at relatively high temperatures, easy yellowing and volatilization loss.With list
Phenolic is compared, and bisphenol type Hinered phenols antioxidant molecular weight is big, not volatile and extraction loss is smaller, anti-aging effect compared with
It is good, many such antioxidant protection effects quite or slightly above secondary diarylamine kind antioxidant.As antioxidant 2246 is being matched
The one third amount that antioxidant 264 need to be only used in side, can meet or exceed the former effect for using antioxidant 264.But
The use cost of polyphenol kind antioxidant is generally higher, though and these antioxidant have the good thermostabilization of antioxygenic property and
Compatibility is not fine, but because causing antioxidant or decomposition product that can move out and will lead to from material in use
The mechanical degradation of plastics.
Summary of the invention
The technical problems to be solved by the invention: it is poor for current polypropylene antioxidant thermostabilization, and compatibility is low
Problem, the present invention provides a kind of preparation methods of polypropylene antioxidant.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of polypropylene antioxidant, the preparation method include the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:22 in mass ratio~30 are subjected to ultrasonic vibration, are put into reactor, carbonic acid is added
The surfactant of the calcium chloride, sodium carbonate quality 6~9% that 1~2 times of sodium quality and the bicarbonate of sodium carbonate quality 2~4%
Ammonium is warming up to 40~50 DEG C, heat preservation；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.6~0.8% is added, is cooled to room temperature, stand, discharging, mistake
Filter is washed, dry, collects dried object, according to parts by weight, take 180~190 parts of water, 50~55 parts of dried objects, 20~26 parts it is mixed
Close monomer, 10~13 portions of activating agents, 4~6 parts of polyethylene glycol, 2~5 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, preheat, adds poly- second
Glycol, initiator heat up, and react, cooling, discharge, freeze-drying, collect freeze-drying object；
(4) it will be freeze-dried object, extract and sulfuric acid solution 7:1~3:10 in mass ratio, ultrasonic vibration heats, and it is cooling, it adjusts
PH is to neutrality, and concentration, collection concentrate is to get polypropylene antioxidant.
Auxiliary agent is ethyl orthosilicate in the step (1), pentaerythritol stearate 6:1~3 in mass ratio mix.
Surfactant is ionic surfactant in the step (1).
The ionic surfactant is Cocoamidopropyl betaine, neopelex, dodecyl two
Any one in methylbenzyl ammonium bromide.
Adjuvant is sodium tripolyphosphate in the step (2), lecithin 4:1~3 in mass ratio mix.
The mix monomer is acrylamide, acrylic acid 4:2~5 in mass ratio mix.
The activating agent the preparation method comprises the following steps: dibromo butene glycol and tetrahydrofuran 1:8~12 in mass ratio are put into appearance
In device, the methylimidazole of dibromo butene glycol quality 70~80% is added, is reacted in 80~85 DEG C of heating, then rotate removal four
Hydrogen furans is to get activating agent.
The initiator is ammonium persulfate, any one in potassium peroxydisulfate.
In the step (4) extract the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:4~8 in mass ratio are mixed,
Mixture is collected, mixture and mixed solvent 1:5~7 in mass ratio are heated, is filtered, filtrate is collected, rotary evaporation is gone
Except mixed solvent, residue is collected to get extract.
The mixed solvent is ethanol solution, 4:3 is mixed acetone by volume.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is mixed by sodium carbonate as raw material with auxiliary agent, by react with calcium chloride, passes through table
The effect of face activating agent and ammonium hydrogen carbonate forms porous nanometer calcium carbonate, is then mixed with mix monomer, forms poly-
Object engrafted nanometer calcium carbonate structure is closed, and by the effect of activating agent, the polymer of formation is modified, forms cation
Living polymer, finally again by being combined with extract, to form polypropylene antioxidant；
(2) present invention in use, can be very good to improve heatproof first by the carrier hole nanometer calcium carbonate formed
Performance, the polymer that secondly carrier is grafted can be very good oxygen radical and react, and interrupt so as to cause its active chain growth,
And then improve can antioxygenic property, and using the substances such as lipid therein for extracting acquisition to Pericarpium Kaki, orange peel, one
Aspect can function well as volatilization diffusion, on the other hand carry out sulfonation processing by sulfuric acid, it is made to have sulfonic acid group,
And containing hindered phenol structure, antioxygenic property can be preferably improved, and passes through the effect of extract and living polymer,
Enhance antioxidant and plastics merges performance.
Specific embodiment
Auxiliary agent is ethyl orthosilicate, pentaerythritol stearate 6:1~3 in mass ratio mix.
Surfactant is ionic surfactant.
Ionic surfactant is Cocoamidopropyl betaine, neopelex, dodecyl dimethyl
Any one in Benzylphosphonium Bromide ammonium.
Adjuvant is sodium tripolyphosphate, lecithin 4:1~3 in mass ratio mix.
Mix monomer is acrylamide, acrylic acid 4:2~5 in mass ratio mix.
Activating agent the preparation method comprises the following steps: dibromo butene glycol and tetrahydrofuran 1:8~12 in mass ratio are put into container,
The methylimidazole for adding dibromo butene glycol quality 70~80% reacts 9h in 80~85 DEG C of heating, then rotates removal tetrahydro
Furans is to get activating agent.
Initiator is ammonium persulfate, any one in potassium peroxydisulfate.
Extract the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:4~8 in mass ratio are mixed, collect mixture, will
Mixture and mixed solvent 1:5~7 in mass ratio carry out heating 5h at 80 DEG C, filter, and collect filtrate, rotary evaporation removal mixing
Solvent collects residue to get extract.
Mixed solvent is 1.6mol/L ethanol solution, 4:3 is mixed acetone by volume.
A kind of preparation method of polypropylene antioxidant, the preparation method include the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:22 in mass ratio~30 are subjected to ultrasonic vibration 20min, are put into reactor, is added
The surfactant of the calcium chloride, sodium carbonate quality 6~9% that 1~2 times of sodium carbonate quality and the carbonic acid of sodium carbonate quality 2~4%
Hydrogen ammonium is warming up to 40~50 DEG C, keeps the temperature 4h；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.6~0.8% is added, is cooled to room temperature, stands 10h, discharges,
Filtering is collected dried object and takes 180~190 parts of water, 50~55 parts according to parts by weight using water washing in 110 DEG C of dry 1h
Dried object, 20~26 parts of mix monomers, 10~13 portions of activating agents, 4~6 parts of polyethylene glycol, 2~5 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, in 40 DEG C of preheating 30min,
Polyethylene glycol, initiator are added, is warming up to 80~85 DEG C, 7h is reacted, is cooled to room temperature, is discharged, freezing is collected in freeze-drying
Dried object；
(4) it will be freeze-dried object, extract and 1.0mol/L sulfuric acid solution 7:1~3:10 in mass ratio, ultrasonic vibration 30min,
60 DEG C are heated to, 1h is heated, it is cooling, pH is adjusted to neutrality, is obtained mixture, is concentrated into the 70~75% of volume of mixture, collects
Concentrate is to get polypropylene antioxidant.
Embodiment 1
Auxiliary agent is ethyl orthosilicate, pentaerythritol stearate 6:1 in mass ratio is mixed.
Surfactant is ionic surfactant.
Ionic surfactant is Cocoamidopropyl betaine.
Adjuvant is sodium tripolyphosphate, lecithin 4:1 in mass ratio is mixed.
Mix monomer is acrylamide, acrylic acid 4:2 in mass ratio is mixed.
Activating agent the preparation method comprises the following steps: dibromo butene glycol and tetrahydrofuran 1:8 in mass ratio are put into container, then plus
The methylimidazole for entering dibromo butene glycol quality 70% reacts 9h in 80 DEG C of heating, then rotates removal tetrahydrofuran to get activity
Agent.
Initiator is ammonium persulfate.
Extract the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:4 in mass ratio are mixed, collect mixture, will mix
Object and mixed solvent 1:5 in mass ratio carry out heating 5h at 80 DEG C, filter, and collect filtrate, and rotary evaporation removes mixed solvent, receive
Collect residue to get extract.
Mixed solvent is 1.6mol/L ethanol solution, 4:3 is mixed acetone by volume.
A kind of preparation method of polypropylene antioxidant, the preparation method include the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:22 in mass ratio are subjected to ultrasonic vibration 20min, are put into reactor, carbonic acid is added
The surfactant of the calcium chloride, sodium carbonate quality 6% that 1 times of sodium quality and the ammonium hydrogen carbonate of sodium carbonate quality 2%, are warming up to 40
DEG C, keep the temperature 4h；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.6% is added, is cooled to room temperature, stands 10h, discharges, filtering,
Using water washing, in 110 DEG C of dry 1h, collect dried object, according to parts by weight, take 180 parts of water, 50 parts of dried objects, 20 parts it is mixed
Close monomer, 10 portions of activating agents, 4 parts of polyethylene glycol, 2 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, in 40 DEG C of preheating 30min,
Polyethylene glycol, initiator are added, is warming up to 80 DEG C, 7h is reacted, is cooled to room temperature, is discharged, freeze-drying is collected in freeze-drying
Object；
(4) object, extract and 1.0mol/L sulfuric acid solution 7:1:10 in mass ratio, ultrasonic vibration 30min, heating will be freeze-dried
To 60 DEG C, 1h is heated, it is cooling, pH is adjusted to neutrality, is obtained mixture, is concentrated into the 70% of volume of mixture, collects concentrate, i.e.,
Obtain polypropylene antioxidant.
Embodiment 2
Auxiliary agent is ethyl orthosilicate, pentaerythritol stearate 6:3 in mass ratio is mixed.
Surfactant is ionic surfactant.
Ionic surfactant is neopelex.
Adjuvant is sodium tripolyphosphate, lecithin 4:3 in mass ratio is mixed.
Mix monomer is acrylamide, acrylic acid 4:5 in mass ratio is mixed.
Activating agent the preparation method comprises the following steps: dibromo butene glycol and tetrahydrofuran 1:12 in mass ratio are put into container, then
The methylimidazole of dibromo butene glycol quality 80% is added, reacts 9h in 85 DEG C of heating, then rotates removal tetrahydrofuran to get work
Property agent.
Initiator is potassium peroxydisulfate.
Extract the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:8 in mass ratio are mixed, collect mixture, will mix
Object and mixed solvent 1:7 in mass ratio carry out heating 5h at 80 DEG C, filter, and collect filtrate, and rotary evaporation removes mixed solvent, receive
Collect residue to get extract.
Mixed solvent is 1.6mol/L ethanol solution, 4:3 is mixed acetone by volume.
A kind of preparation method of polypropylene antioxidant, the preparation method include the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:30 in mass ratio are subjected to ultrasonic vibration 20min, are put into reactor, carbonic acid is added
The surfactant of the calcium chloride, sodium carbonate quality 9% that 2 times of sodium quality and the ammonium hydrogen carbonate of sodium carbonate quality 4%, are warming up to 50
DEG C, keep the temperature 4h；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.8% is added, is cooled to room temperature, stands 10h, discharges, filtering,
Using water washing, in 110 DEG C of dry 1h, collect dried object, according to parts by weight, take 190 parts of water, 55 parts of dried objects, 26 parts it is mixed
Close monomer, 13 portions of activating agents, 6 parts of polyethylene glycol, 5 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, in 40 DEG C of preheating 30min,
Polyethylene glycol, initiator are added, is warming up to 85 DEG C, 7h is reacted, is cooled to room temperature, is discharged, freeze-drying is collected in freeze-drying
Object；
(4) object, extract and 1.0mol/L sulfuric acid solution 7:3:10 in mass ratio, ultrasonic vibration 30min, heating will be freeze-dried
To 60 DEG C, 1h is heated, it is cooling, pH is adjusted to neutrality, is obtained mixture, is concentrated into the 75% of volume of mixture, collects concentrate, i.e.,
Obtain polypropylene antioxidant.
Embodiment 3
Auxiliary agent is ethyl orthosilicate, pentaerythritol stearate 6:2 in mass ratio is mixed.
Surfactant is ionic surfactant.
Ionic surfactant is dodecyl dimethyl benzyl ammonium bromide.
Adjuvant is sodium tripolyphosphate, lecithin 4:2 in mass ratio is mixed.
Mix monomer is acrylamide, acrylic acid 4:3 in mass ratio is mixed.
Activating agent the preparation method comprises the following steps: dibromo butene glycol and tetrahydrofuran 1:10 in mass ratio are put into container, then
The methylimidazole of dibromo butene glycol quality 75% is added, reacts 9h in 83 DEG C of heating, then rotates removal tetrahydrofuran to get work
Property agent.
Initiator is ammonium persulfate.
Extract the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:6 in mass ratio are mixed, collect mixture, will mix
Object and mixed solvent 1:6 in mass ratio carry out heating 5h at 80 DEG C, filter, and collect filtrate, and rotary evaporation removes mixed solvent, receive
Collect residue to get extract.
Mixed solvent is 1.6mol/L ethanol solution, 4:3 is mixed acetone by volume.
A kind of preparation method of polypropylene antioxidant, the preparation method include the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:26 in mass ratio are subjected to ultrasonic vibration 20min, are put into reactor, carbonic acid is added
The surfactant of the calcium chloride, sodium carbonate quality 7% that 1.5 times of sodium quality and the ammonium hydrogen carbonate of sodium carbonate quality 3%, are warming up to
45 DEG C, keep the temperature 4h；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.7% is added, is cooled to room temperature, stands 10h, discharges, filtering,
Using water washing, in 110 DEG C of dry 1h, collect dried object, according to parts by weight, take 185 parts of water, 52 parts of dried objects, 25 parts it is mixed
Close monomer, 12 portions of activating agents, 5 parts of polyethylene glycol, 3 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, in 40 DEG C of preheating 30min,
Polyethylene glycol, initiator are added, is warming up to 82 DEG C, 7h is reacted, is cooled to room temperature, is discharged, freeze-drying is collected in freeze-drying
Object；
(4) object, extract and 1.0mol/L sulfuric acid solution 7:2:10 in mass ratio, ultrasonic vibration 30min, heating will be freeze-dried
To 60 DEG C, 1h is heated, it is cooling, pH is adjusted to neutrality, is obtained mixture, is concentrated into the 73% of volume of mixture, collects concentrate, i.e.,
Obtain polypropylene antioxidant.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking extract.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking activating agent.
Comparative example 3: the polypropylene antioxidant of Shanghai City company production.
The polypropylene antioxidant that above-described embodiment is obtained with comparative example is detected, is added into high-speed mixer
The polypropylene antioxidant that 50g polypropylene, 0.15g embodiment and comparative example obtain, high-speed stirred 10min, discharging use screw rod
Extruder is granulated, and will be made to obtain particle survey oxidation induction period, is molded member, does mechanics properties testing, do thermo-oxidative ageing test, aoxidize
Induction period: using DSC200PC type differential scanning calorimetric analysis instrument, and the sample that quality is (15.0 ± 0.5) mg is placed in aluminum dish,
Lead to people's nitrogen with (50 ± 5) mL/min, controls 20 DEG C/min of heating rate, be warming up to 160 DEG C.Constant temperature 3min, uses replacement of oxygen
Nitrogen, 160 DEG C of constant temperature, until exothermic maximum signal occurs, the time of record is oxidation induction period min.Hot air aging
Test:
Sample is contained with aluminum dish, thickness is about 5mm, and it is put into LR016A type thermo-oxidative ageing case and carries out air oven aging test,
180 DEG C of senile experiment temperature of setting sets ventilation condition, and the appearance color situation of change of particle is observed in timing, when particle becomes
Time min is recorded when dark brown, is set as scorch time, the longer sample of scorch time shows that antioxygen property is all right, in basis
GB1040-92 detects the tensile strength of particle, obtains that the results are shown in Table 1.
Table 1:
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Oxidation induction period/min | 85 | 83 | 80 | 76 | 73 | 62 |
| Scorch time/min | 356 | 354 | 352 | 339 | 322 | 226 |
| Tensile strength/MPa | 40 | 39 | 38 | 27 | 26 | 16 |
In summary, polypropylene antioxidant effect of the invention is more preferable as can be seen from Table 1, is worth of widely use, the above institute
Preferred mode only of the invention is stated, is not intended to limit the invention, all within the spirits and principles of the present invention, made
What modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of polypropylene antioxidant, which is characterized in that the preparation method includes the following steps:
(1) sodium carbonate, auxiliary agent and water 7:1:22 in mass ratio~30 are subjected to ultrasonic vibration, are put into reactor, carbonic acid is added
The surfactant of the calcium chloride, sodium carbonate quality 6~9% that 1~2 times of sodium quality and the bicarbonate of sodium carbonate quality 2~4%
Ammonium is warming up to 40~50 DEG C, heat preservation；
(2) after wait keep the temperature, the adjuvant of sodium carbonate quality 0.6~0.8% is added, is cooled to room temperature, stand, discharging, mistake
Filter is washed, dry, collects dried object, according to parts by weight, take 180~190 parts of water, 50~55 parts of dried objects, 20~26 parts it is mixed
Close monomer, 10~13 portions of activating agents, 4~6 parts of polyethylene glycol, 2~5 parts of initiators；
(3) water, dried object, mix monomer and activating agent are put into reaction kettle first, nitrogen protection, preheat, adds poly- second
Glycol, initiator heat up, and react, cooling, discharge, freeze-drying, collect freeze-drying object；
(4) it will be freeze-dried object, extract and sulfuric acid solution 7:1~3:10 in mass ratio, ultrasonic vibration heats, and it is cooling, it adjusts
PH is to neutrality, and concentration, collection concentrate is to get polypropylene antioxidant.
2. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that auxiliary agent in the step (1)
It is mixed for ethyl orthosilicate, pentaerythritol stearate 6:1~3 in mass ratio.
3. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that surface in the step (1)
Activating agent is ionic surfactant.
4. the preparation method of polypropylene antioxidant according to claim 3, which is characterized in that the ionic surfactant
Agent is Cocoamidopropyl betaine, neopelex, any one in dodecyl dimethyl benzyl ammonium bromide.
5. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that auxiliary in the step (2)
Agent is sodium tripolyphosphate, lecithin 4:1~3 in mass ratio mix.
6. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that the mix monomer is propylene
Amide, acrylic acid 4:2~5 in mass ratio mix.
7. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that the preparation side of the activating agent
Method are as follows: dibromo butene glycol and tetrahydrofuran 1:8~12 in mass ratio are put into container, add dibromo butene glycol quality
70~80% methylimidazole is reacted in 80~85 DEG C of heating, then rotates removal tetrahydrofuran to get activating agent.
8. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that the initiator is persulfuric acid
Any one in ammonium, potassium peroxydisulfate.
9. the preparation method of polypropylene antioxidant according to claim 1, which is characterized in that extracted in the step (4)
Object the preparation method comprises the following steps: Pericarpium Kaki, orange peel 4:4~8 in mass ratio are mixed, collect mixture, by mixture with mix
Solvent 1:5~7 in mass ratio are heated, filtering, collect filtrate, rotary evaporation remove mixed solvent, collect residue to get
Extract.
10. the preparation method of polypropylene antioxidant according to claim 9, which is characterized in that the mixed solvent is second
4:3 is mixed by volume for alcoholic solution, acetone.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444527A (en) * | 2021-06-29 | 2021-09-28 | 江苏品和石油科技有限公司 | Preparation method of antioxidant stabilizer for lithium ion diaphragm pore-forming oil |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444527A (en) * | 2021-06-29 | 2021-09-28 | 江苏品和石油科技有限公司 | Preparation method of antioxidant stabilizer for lithium ion diaphragm pore-forming oil |
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