CN106519500A - Standard substance for phthalic acid ester plasticizer measurement and preparation method of standard substance - Google Patents
Standard substance for phthalic acid ester plasticizer measurement and preparation method of standard substance Download PDFInfo
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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Abstract
The invention belongs to the field of compositions of high-molecular compounds, and provides a standard substance for phthalic acid ester plasticizer measurement and a preparation method of the standard substance. The standard substance for phthalic acid ester plasticizer measurement is prepared from a phthalic acid ester plasticizer, polyvinyl chloride resin, a main plasticizer, a heat stabilizer, a lubricating agent and an antioxidant. The ingredients of the standard substance for phthalic acid ester plasticizer measurement is high in designability, and the content of all the ingredients is adjusted, so that the standard substance for phthalic acid ester plasticizer measurement is high in uniformity and good in stability. By means of the standard substance for phthalic acid ester plasticizer measurement, a phthalic acid ester plasticizer in a PVC food contact material is measured more conveniently and faster, and meanwhile the accuracy of the detecting result is improved.
Description
Technical field
The invention belongs to the compositions field of macromolecular compound, more particularly to a kind of survey of phthalic ester plasticizer
Surely with standard items and preparation method thereof.
Background technology
Polyvinyl chloride (PVC) is one of utilization rate highest plastic packing bag, is often commonly used by people for packaging heating food,
Such as deep-fried twisted dough sticks, cake, meat and cooked food class etc. are containing the high food of grease.It is plastic to increase which in the production of polyvinyl chloride packaging material
Property and intensity, improve its transparency, need to add various plasticizer, wherein using more generally phthalic acid ester.In PVC
In class flexible article, particularly preservative film need to typically add 40%～50%.Most of food are carried out interior using plastic products
Packaging or liner, phthalate compound then may contain fatty foods to food, particularly from plastic packaging bag, such as
Migrate in milk, meat, the time that food is stored in plastic package material is longer, or in the plastic material of packaged food
Plasticizer loading is higher, can all increase the amount that plasticizer is migrated in food, i.e., bigger to the pollution level of food.Additionally, adjacent
Phthalates compound is the important environmental hormone class material of a class, can affect the endocrine system of the mankind and wild animal
System, causes reproduction, development and abnormal behavior.
China has strict regulation in terms of food packaging material, and such as GB 9685-2008 define food contact to be held
DMP, DIBP, DBP, DEHP, DINP, DAP, DIOP and diallyl phthalate and acrylic acid second used in device, material
The highest usage amount of 8 kinds of phthalic ester plasticizers of co-polymer of ester and methacrylic acid；GB/T 21928-2008
Define phthalic acid two (2- methoxyl groups) ester, diphenyl phthalate, dinonyl phthalate, phthalic acid two
The detection method of 16 kinds of phthalic acid esters such as (2- methoxyl groups) ester.European Union 2002/72/EC and 2007/19/EC and new issue
REGULATION (EU) No10/2011 allow DBP, DEHP, DINP, DAP, DIDP, BBP used in food contact material and
7 kinds of phthalic ester plasticizers such as NDOP+DDP mixtures and give migration limitation；The U.S.
FDA21cfr178.3740 etc. allows to use DHXP, DCHP, DINP, BBP and phthalic acid two in indirect food additive
5 kinds of phthalic ester plasticizers such as phenyl ester, wherein 4 kinds give migration limitation.
Therefore, develop phthalic ester plasticizer measure standard items to detect for phthalic ester plasticizer
The comparison of data, the Accuracy Verification of detection method, the meaning of the calibration of detecting instrument and the quality control of test result and examination
Justice is great.
The content of the invention
The technical problem to be solved is to provide a kind of phthalic ester plasticizer measure standard items
And preparation method thereof, it is intended to make the detection of phthalic ester plasticizer in material more convenient, while improving the standard of detection
True property.
The present invention is achieved in that a kind of phthalic ester plasticizer measure standard items, the O-phthalic
Acid ester type plasticizer measure standard items include following components by weight percentage：
Further, the phthalic ester plasticizer include DEHP, DBP, DMEP, DBEP, DPHP, DIPRP and
BBP。
Further, the main plasticiser be ATBC, trioctyl trimellitate (TOTM), epoxidized soybean oil,
At least one in dioctyl adipate and triphenyl phosphite.
Further, the heat stabilizer includes lead stearate, calcium stearate, zinc stearate, maleic acid dioctyltin
With at least one in the different monooctyl ester dioctyltin of two Thioglycolic acids.
Further, the lubricant includes at least one in EBS, ACR, chlorinated paraffin and butyl stearate.
Further, the antioxidant includes four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrite
Ester, 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), three [2.4- di-tert-butyl-phenyls] phosphite esters and phosphorous acid three
At least one in phenyl ester.
Present invention also offers the preparation method of above-mentioned phthalic ester plasticizer measure standard items, including with
Lower step：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant are weighed, detection is sampled；
Above-mentioned each raw material is mixed with phthalic ester plasticizer, mixture is obtained；
The mixture is carried out into melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and is adopted
Granulated with hot cut method, obtain micelle；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps.
Further, the temperature during mixing is 85-95 DEG C, and rotating speed is 1200 revs/min, mixes 60-120 minutes.
Further, the pan feeding section temperature of the melting extrusion is 130-150 DEG C, and compression section temperature is 140-160 DEG C,
It is 155-175 DEG C to change section temperature, and screw speed is 50-85 rev/min, and fervent rotating speed is 50-120 rev/min.
Further, the rotating speed of the mixed at high speed is 800 revs/min, and the time is 10-20 minutes.
Compared with prior art, beneficial effect is the present invention：Phthalate provided in an embodiment of the present invention increases
Modeling agent measure standard items, composition designability are strong, by adjusting each component content, make the phthalate plasticising of acquisition
The uniformity of agent measure standard items is high, good stability.The phthalic ester plasticizer measure standard items are made to PVC
In food contact material, the measure of phthalic ester plasticizer is more convenient, while improve the accurate of its testing result
Property.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
Embodiments provide a kind of phthalic ester plasticizer measure standard items, the phthalic acid
Ester plasticizer measure standard items include following components by weight percentage：
Phthalic ester plasticizer measure standard items provided in an embodiment of the present invention, composition designability are strong, lead to
Cross and adjust each component content, make the uniformity of the phthalic ester plasticizer measure standard items of acquisition high, good stability.
Connected by hydrogen bond and Van der Waals force between phthalic ester plasticizer and plastic molecules, retain each relatively independent each other
Chemical property, phthalic ester plasticizer are easier to move in environment from plastics.The phthalate plasticising
Agent measure standard items are measured to the content of phthalic ester plasticizer in PVC food contact materials, can make survey
Determine that process is more convenient, while improve the accuracy of its testing result.
Specifically, the phthalic ester plasticizer include phthalic acid two (2- ethylhexyls) ester (DEHP),
Dibutyl phthalate (DBP), phthalic acid two (2- methoxyl groups) ester (DMEP), butyl cellosolve phthalate
(DBEP), diphenyl phthalate (DPHP), diisopropyl phthalate (DIPRP) and phthalic acid fourth Bian ester
(BBP).The Corvic can be with other plurality of raw materials, such as plasticizer, filler and other polymer-compatibles.
The main plasticiser is that ATBC, trioctyl trimellitate (TOTM), epoxidized soybean oil, adipic acid two are pungent
At least one in ester and triphenyl phosphite.The primary plasticizer goes out when GC-MS detects (gas chromatography-mass spectrum detection)
Peak time is after 7 kinds of phthalic acid ester plasticisers or appearance time appearance time weight not with phthalic acid ester plasticiser
Folded, noiseless ion, will not produce interference to the accuracy of object phthalic acid ester test.
The heat stabilizer includes that lead stearate, calcium stearate, zinc stearate, maleic acid dioctyltin and two dredge base second
At least one in the different monooctyl ester dioctyltin of acid.The heat stabilizer is used as standard items processing heat stability auxiliary agent.Polychlorostyrene second
The heat endurance of olefine resin is poor, and the use of the additive such as main plasticiser, lubricant can change outside the physics of polyvinyl chloride (PVC)
See and operating characteristic, but the decomposition of polymer can not be prevented.In (such as heat, radiation) and (oxygen, ozone) factor of chemistry of physics
Effect is lower to make each polymeric material of the standard items gradually decompose, and the stabilizer can effectively be prevented, reduces or be stopped
The degraded of each polymeric material in the standard items.
The lubricant includes at least one in EBS, ACR, chlorinated paraffin and butyl stearate.The lubricant conduct
Standard items processing and lubrication auxiliary agent.High polymer after melting have higher viscosity, in process, the high polymer of melting
When by runners such as narrow slit, cast gates, polymer melt will produce friction with processing equipment surface, and some frictions are to polymer
Processing be very unfavorable, these frictions reduce fluidity of molten, while serious friction can make film surface become coarse,
Lack gloss or flow liner occur.The lubricant can improve lubricity, reduce friction, reduces Interface Adhesion performance.Additionally, institute
State lubricant and can improve mobility, play melting accelerator, prevent adhesion and antistatic agent, slipping agent etc. are acted on.
The antioxidant includes that four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester is (anti-oxidant
Agent 1010), 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols) (antioxidant 2246), three [2.4- di-tert-butyl-phenyls]
At least one in phosphite ester (antioxidant 168) and triphenyl phosphite.The antioxidant is anti-as standard items processing
Oxidation promoter.In manufacture, processing, storage and application process, it is anti-that polymeric material therein oxidation to the standard items can occur
Answer and cause material degradation or crosslinking, so as to change the performance of material.The oxidizing process of the polymeric material is free radical type
Chain reaction, the plastics antioxidant can capture reactive radical species, generate nonactive free radical, or can decompose
The polymer hydroperoxides produced in oxidizing process, terminate chain reaction, so as to delay the oxidation of the polymeric material
Process, enables polymeric material to be smoothed out processing, and increases the service life.
In phthalic ester plasticizer measure standard items provided in an embodiment of the present invention, by optimizing each component institute
Use concrete material, make the phthalic ester plasticizer measure standard items stability high, with thermal ageing resistant performance it is high,
Meet melting extrusion technique needs repeatedly and the advantages of each component is not separated out.
The embodiment of the present invention additionally provides the preparation method of above-mentioned phthalic ester plasticizer measure standard items,
Comprise the following steps：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant are weighed, detection is sampled, with true
Protect above-mentioned raw materials and do not detect target compound phthalic ester plasticizer；
Above-mentioned each raw material is mixed with phthalic ester plasticizer, mixture is obtained；
The mixture is carried out into melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and is adopted
Granulated with hot cut method, obtain micelle；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps.
The preparation method of the phthalic ester plasticizer measure standard items that the embodiment of the present invention is also provided, using height
Speed mixing, the mode that melting mixing expressing technique combines repeatedly, process are simple, make obtained standard sample uniformity high, steady
It is qualitative good.Additionally, the preparation method overcomes traditional single melting extrusion technique and blowing is prepared in sample technique, it is guarantor
The uniformity of card sample, it is necessary to give up the shortcoming extruded front 1/5 and rear 1/5 part of finished product, only stay the product of mid portion.It is logical
It is columned to cross the phthalic ester plasticizer measure standard items that the preparation method of the embodiment of the present invention prepares
Particle, many of phthalic ester plasticizer content are 0.05mg/kg～50.0mg/kg.
Specifically, the temperature during mixing is 85-95 DEG C, and rotating speed is 1200 revs/min, mixes 60-120 minutes.
The pan feeding section temperature of the melting extrusion is 130-150 DEG C, and compression section temperature is 140-160 DEG C, homogenizing zone temperature
For 155-175 DEG C, screw speed is 50-85 rev/min, and fervent rotating speed is 50-120 rev/min.
The rotating speed of the mixed at high speed is 800 revs/min, and the time is 10-20 minutes.
The embodiment of the present invention makes the phthalic acid for preparing by being optimized to each design parameter in preparation process
Ester plasticizer standard sample has corresponding function.Phthalic ester plasticizer standard sample prepared by the present invention is suitable for
In laboratory monitoring plastics, the quality evaluation of the work of detection containing phthalic ester plasticizer, Laboratory Accreditation and ability are tested
Card, be also applied for measuring method evaluation, tester is examined and uncertainty of measurement evaluation etc..
Embodiment
With gross weight, as 5kg, as a example by 7 kinds of phthalic acid ester contents formula respectively as 5.0mg/kg, (concentration range is
0.05-50.0mg/kg), a kind of phthalic ester plasticizer standard sample, its component include：
Corvic：3.065kg；
Calcium stearate：0.2kg；
Zinc stearate：0.1kg
Butyl stearate：0.1kg
Trioctyl trimellitate (TOTM)：1.5kg
Antioxidant 1010：2.5g；
Antioxidant 168：2g
DEHP, DBP, DMEP, DBEP, DPHP, DIPRP and BBP are 25.0mg.
The preparation method is as follows：
Weigh 3.065kg polyvinyl chloride and be added to high-speed mixer, then weigh calcium stearate 0.2kg, zinc stearate 0.1kg
And butyl stearate 0.1kg mixes 10 minute by 50r/min with polyvinyl chloride；
Weigh each 25.0mg of target compound DEHP, DBP, DMEP, DBEP, DPHP, DIPRP and BBP put into it is at a high speed mixed
In conjunction machine, the heating of high-speed mixer chuck is opened, temperature setting is 90 DEG C, the mixed at high speed 120 under 1200 revs/min of rotating speed
Minute；
The material powder feed machine being well mixed is entered by 25-55 rev/min of rate of feeding input double screw extruder
Row melting extrusion, is granulated using hot cut method, and technological parameter is as follows：Pan feeding section 130-150 DEG C, 140-160 DEG C of compression section, homogenizing zone
155-175 DEG C, 50-85 rev/min of screw speed, 50-120 rev/min of fervent rotating speed；
The micelle produced is put in high-speed mixer, under 800 revs/min of rotating speed after mixed at high speed 10-20 minute
By above-mentioned steps, melting extrusion is granulated 6 times repeatedly, you can the uniform and stable mark of target compound phthalic acid ester is obtained
Quasi- sample.
Uniformity testing is carried out to above standard sample：
(1) at least 0.1 ± 0.005g samples are weighed, is put in the flat screw socket bottle of 40mL browns.Add 10mL tetrahydrofurans
Into brown bottle.In supersonic cleaning machine, ultrasound makes sample fully dissolve in 60 minutes.20mL n-hexanes are added to make polyvinyl chloride
(PVC) polymer Precipitation.Shaking and stand at least 5 minutes makes polymer Precipitation.
By 0.45 μm of membrane filter filtering solution, a small amount of filtrate is collected in independent sample bottle, tested for GC-MS.
(2) GC-MS test conditions：
Chromatographic column：DB-5HT, 30m*250 μm * 0.25 μm；
Carrier gas：Helium, flow:1mL/min；
Injector temperature:280℃；
Sampling volume：1μL；
Input mode:Do not shunt；
Interface temperature：280℃；
Ionization mode：EI；
Heating schedule：60 DEG C of holding 1min, 20 DEG C/min heating rates rise to 220 DEG C from 60 DEG C, keep 1min, then with 5
DEG C 280 DEG C are risen to, keep 4min.
Scanning of the mass spectrum parameter：TIC (TIC) is qualitative, mass scan range：M/z 50～500.Select from
Son monitoring (SIM) is quantitative, selects ion scan to arrange.
(3) result of calculation：
Standard working curve, GC-MS Chemstation softwares are set up further according to known concentration of standard solution and response
Automatically calculating solution concentration result computing formula according to the response of sample is：
Phthalic acid ester content (m/m)=C*V*D/W (unit mg/kg).
C：GC-MS instrument tests 1.3.5 solution phthalic acid lipid concentration (unit mg/L)；
V：Tetrahydrofuran and the cumulative volume (Unit/mL) of n-hexane that phthalic acid ester extraction pre-treatment is added；
D：GC-MS examination with computer dilution gfactors, the D=1 if undiluted；
W：Weight (the unit g) of sample.
(4) calibration standard solution concentration
The preparation of standard liquid adopts stepwise dilution method, first pipettes the standard substance solution of 2.5mL, is settled to 25mL, matches somebody with somebody
The storing solution of 100mg/L is made, storing solution stepwise dilution concentration in table 1 is recycled, calibration curve is obtained.
1 calibration standard solution concentration of table
| Analytes | Standard1 | Standard2 | Standard3 | Standard4 | Standard5 |
| 7P | 1mg/L | 2mg/L | 5mg/L | 10mg/L | 20mg/L |
Phthalic acid ester mark sample tests：
Measurement result carries out data statistic analysis using variance statistic method.Jing statistical computations, it is adjacent in standard substance sample
The uniformity testing result of phthalic acid ester is as shown in table 4 below, and in all standard substance samples, the F values of phthalic acid ester are little
In F0.05, (24,25)=1.96, multinomial phthalic acid ester has good uniformity in the standard substance sample, uniformity testing
Method is sampled as 0.1g, final to determine that standard substance minimum sample mass is 0.1g.The uniformity testing of each phthalic acid ester
Result of calculation in detail see the table below.
2 standard sample DEHP uniformity testing results (mg/kg) of table
3 standard sample DBP uniformity testing results (mg/kg) of table
4 standard sample DBEP uniformity testing results (mg/kg) of table
5 standard sample DMEP uniformity testing results (mg/kg) of table
6 standard sample DPHP uniformity testing results (mg/kg) of table
7 standard sample DIPRP assays (mg/kg) of table
8 standard sample BBP assays (mg/kg) of table
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of phthalic ester plasticizer measure standard items, it is characterised in that the phthalate plasticising
Agent measure standard items include following components by weight percentage：
2. phthalic ester plasticizer measure standard items as claimed in claim 1, it is characterised in that the adjacent benzene two
Formate ester plasticizer includes DEHP, DBP, DMEP, DBEP, DPHP, DIPRP and BBP.
3. phthalic ester plasticizer measure standard items as claimed in claim 1, it is characterised in that the main plasticizing
During agent is ATBC, trioctyl trimellitate (TOTM), epoxidized soybean oil, dioctyl adipate and triphenyl phosphite
At least one.
4. phthalic ester plasticizer measure standard items as claimed in claim 1, it is characterised in that described thermally-stabilised
Agent includes the different monooctyl ester dioctyltin of lead stearate, calcium stearate, zinc stearate, maleic acid dioctyltin and two Thioglycolic acids
In at least one.
5. phthalic ester plasticizer measure standard items as claimed in claim 1, it is characterised in that the lubricant
Including at least one in EBS, ACR, chlorinated paraffin and butyl stearate.
6. phthalic ester plasticizer measure standard items as claimed in claim 1, it is characterised in that described anti-oxidant
Agent include four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-terts
Butylphenol), at least one in three [2.4- di-tert-butyl-phenyls] phosphite ester and triphenyl phosphite.
7. the preparation method of the phthalic ester plasticizer measure standard items as described in claim 1 to 6 any one,
Characterized in that, comprising the following steps：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant are weighed, detection is sampled；
Above-mentioned each raw material is mixed with phthalic ester plasticizer, mixture is obtained；
The mixture is carried out into melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and using heat
Cutting method is granulated, and obtains micelle；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps.
8. preparation method as claimed in claim 7, it is characterised in that the temperature during mixing is 85-95 DEG C, rotating speed is
1200 revs/min, mix 60-120 minutes.
9. preparation method as claimed in claim 7, it is characterised in that the pan feeding section temperature of the melting extrusion is 130-150
DEG C, compression section temperature is 140-160 DEG C, and homogenizing zone temperature is 155-175 DEG C, and screw speed is 50-85 rev/min, is earnestly turned
Speed is 50-120 rev/min.
10. preparation method as claimed in claim 7, it is characterised in that the rotating speed of the mixed at high speed is 800 revs/min, when
Between be 10-20 minutes.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
| CN109142608A (en) * | 2018-10-22 | 2019-01-04 | 深圳出入境检验检疫局工业品检测技术中心 | A kind of measuring method of four classes, 34 kinds of plasticizer |
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| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
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| CN110887906A (en) * | 2019-11-25 | 2020-03-17 | 贵州省产品质量监督检验院 | Method for rapidly determining epoxidized soybean oil in food |
| CN114381074A (en) * | 2021-12-27 | 2022-04-22 | 国高材高分子材料产业创新中心有限公司 | Standard substance with glass transition temperature lower than 100 ℃ and preparation method thereof |
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