CN108276648B - Polyethylene plastic evaporation residue standard sample master batch particles for food packaging and preparation method thereof - Google Patents
Polyethylene plastic evaporation residue standard sample master batch particles for food packaging and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
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Abstract
The invention discloses a formula of master batch of standard sample of polyethylene plastic evaporation residue for food packaging and a preparation method thereof, wherein the master batch particles of the standard sample of polyethylene plastic evaporation residue are prepared by taking base material LDPE resin, inorganic opening agent calcium carbonate, 1076 antioxidant, diffusant polyethylene wax, lubricant zinc stearate and processing aid fluorinated elastomer PPA as raw materials, and then sequentially carrying out stirring and mixing, primary melting and mixing extrusion granulation, secondary melting and mixing extrusion granulation and third melting and mixing extrusion granulation to finally prepare the master batch particles of the standard sample with the particle size of about 2mm Evaluation of measurement uncertainty, assessment of personnel training and the like.
Description
Technical Field
The invention relates to a formula of standard sample master batch particles and a preparation method thereof, in particular to polyethylene plastic evaporation residue standard sample master batch particles for food packaging and a preparation method thereof.
Background
In the age of food detection, food safety is gradually rising, and the influence of food contact materials on food safety is also a focus of attention of various food manufacturers and consumers. Meanwhile, the evaporation residues are also listed as key detection items for food contact material market admission and export of packaging materials in various countries, and in news of various industries, messages that various food contact materials are exposed, withheld or returned due to unqualified evaporation residues can be often seen. The evaporation residue is an index for detecting the amount of chemical substances possibly separated out when the food contact material contacts with foods such as water, acidic substances, alcohol, grease and the like in the using process, namely, the evaporation residue is used for checking the total amount of the substances in the package migrating to the foods within a certain time. The evaporation residue item is unqualified, which shows that a large amount of residue can be separated out when the product is used in liquor, vinegar, oil and other liquids, and the evaporation residue is harmful to health when the human body excessively absorbs the evaporation residue; in addition, the evaporation residue can directly affect the eating quality of the food, such as color, aroma, taste and the like. Currently, the EU of the European Union, LFGB of Germany, DGCCRF of France, JFSL370 of Japan, FDA of the United states, GU283 of Italy and GB/T5009 of China all make detailed and strict regulations on the evaporation residue index of food contact materials.
A series of detection standards of evaporation residues are provided at home and abroad, and GB/T5009.60, GB5009.69, GB/T5009.203, GB 11679, FDA 1770, EN1186 and the like exist. However, only the test method does not have a corresponding standard sample, the pretreatment and test technologies of the existing methods are different, the test results of different methods for the same sample have larger difference, and the selection of the detection standard of the evaporation residues is troubled. According to the situation, a standard sample of the plastic evaporation residue for food packaging is developed so as to provide reference for verification, comparison and research and development of the evaporation residue detection method. The standard sample can be used for detection requirements of entry and exit detection laboratories, commercial detection laboratories and quality technology supervision laboratories and self-inspection automatic control of production enterprises. Corresponding to import and export inspection of related products such as food contact materials, food packages and the like at present, the method is favorable for ensuring the establishment and utilization of related detection methods in China, verifying the accuracy, reliability and comparability of the methods, and can ensure that mass production and export enterprises can make response work in all aspects such as detection as soon as possible, so that the related products meet the regulatory requirements and detection requirements of Germany LFGB, American FDA, European Union 2002/72/EC instruction, Japanese food sanitation law and the like, the trade is ensured to be carried out smoothly, and the method has large market scale and remarkable economic benefit.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the master batch particles which are suitable for preparing the standard sample of the polyethylene plastic evaporation residue for food packaging and have simple preparation process and the preparation method thereof.
The technical problem of the invention is realized by the following technical scheme:
a polyethylene plastic evaporation residue standard sample master batch particle for food packaging is prepared from the following raw materials in parts by weight:
75-85 parts of base material LDPE resin
19-21 parts of inorganic opening agent calcium carbonate
1076 and 0.05 to 0.15 portion of antioxidant
0.05-0.15 part of dispersing agent polyethylene wax
0.1-0.3 part of lubricant zinc stearate
0.05-0.15 part of PPA (fluorinated elastomer) serving as a processing aid.
The density of the master batch particles of the standard sample is 1.0547g/cm3The melt mass flow rate MFR was 2.472g/10 min.
A preparation method of master batch particles of a standard sample of polyethylene plastic evaporation residues for food packaging comprises the following steps:
accurately weighing the raw materials according to the weight parts, pouring the weighed inorganic opening agent calcium carbonate, 1076 antioxidant, diffusant polyethylene wax, lubricant zinc stearate and processing aid fluorinated elastomer PPA into a high-speed stirrer, and uniformly mixing with the base material LDPE resin;
secondly, putting the uniformly mixed materials into a double-screw extruder for melt mixing extrusion and water-cooling brace forming, then air-drying and cooling, and then drawing the materials into a granulator for granulation forming to prepare primary sample particles;
thirdly, putting the primary sample particles prepared in the second step into a high-speed stirrer for re-mixing, and sequentially carrying out second melting, mixing, extruding, air-drying, cooling, granulating and forming to prepare secondary sample particles;
fourthly, putting the secondary sample particles prepared in the third step into a high-speed stirrer for mixing again, and sequentially carrying out third melting mixing extrusion, air drying cooling and grain cutting molding to prepare standard sample master batch particles;
fifthly, subpackaging the standard sample master batch particles prepared in the step IV into plastic bags, and drying at room temperature and storing in a sealed manner.
In the second step, the screw of the double screw extruder is cleaned by using the base material LDPE resin and fed in a trial mode, and after the extruded and molded material strip is smooth and free of impurities and no black particles are produced at the grain cutting position, the material is fed in a formal mode.
In the first step, a high-speed stirrer for uniformly mixing the raw materials is heated to 70 ℃ and is mixed for 60 minutes at a high speed at a rotating speed of 1200 revolutions per minute; in the third step and the fourth step, the high-speed stirrer is heated to 70 ℃ and is mixed for 20 minutes at a high speed of 1000 revolutions per minute.
In the second step, when the uniformly mixed raw materials are put into the twin-screw extruder, the temperature of the twin-screw extruder is set as follows: 1 stage 130 ℃; 2, 150 ℃; 3, 160 ℃ in section; 4, 160 ℃ in section; the temperature of the machine head is 150 ℃; the screw rotating speed of the double-screw extruder is 230 r/min, and the screw diameter is 30 mm.
And in the second step, the brace is formed through water cooling by a water tank, and is pulled to a granulator after being dried by blowing to complete granulation.
The particle size of the master batch particles of the standard sample prepared in the step (iv) is 2 mm.
And drying the master batch particles of the standard sample in a blowing drying hopper at the temperature of 80 ℃ for 2 hours, and then directly carrying out injection molding.
The high-speed stirrer is a Beijing intet GH-50 high-speed stirrer; the twin-screw extruder is a ZSK-30 twin-screw extruder of Germany WP company.
Compared with the prior art, the invention mainly provides the standard sample master batch particles which are prepared by taking base material LDPE resin, inorganic opener calcium carbonate, 1076 antioxidant, diffusant polyethylene wax, lubricant zinc stearate and processing aid fluorinated elastomer PPA as raw materials and sequentially carrying out stirring and mixing, primary melting, mixing, extruding and granulating, secondary melting, mixing, extruding and granulating and third melting, mixing, extruding and granulating.
Detailed Description
A polyethylene plastic evaporation residue standard sample master batch particle for food packaging is mainly prepared from the following raw materials in parts by weight:
75-85 parts of base material LDPE resin
19-21 parts of inorganic opening agent calcium carbonate
1076 and 0.05 to 0.15 portion of antioxidant
0.05-0.15 part of dispersing agent polyethylene wax
0.1-0.3 part of lubricant zinc stearate
0.05-0.15 part of PPA (fluorinated elastomer) as processing aid
The master batch particles of the standard sample of the polyethylene plastic evaporation residues for food packaging can be prepared according to the weight parts of the raw materials of the three embodiments, and specifically comprise the following components:
the first embodiment,
75 portions of LDPE resin as base material
19 parts of inorganic opening agent calcium carbonate
1076 antioxidant 0.05 part
0.05 part of polyethylene wax serving as a dispersing agent
0.1 part of lubricant zinc stearate
0.05 part of PPA (fluorinated elastomer) as processing aid
Example II,
80 portions of base material LDPE resin
20 parts of inorganic opening agent calcium carbonate
1076 antioxidant 0.1 part
0.1 part of polyethylene wax serving as a dispersing agent
0.2 portion of lubricant zinc stearate
0.1 part of PPA (fluorinated elastomer) as processing aid
Example III,
85 portions of base material LDPE resin
21 parts of inorganic opening agent calcium carbonate
1076 antioxidant 0.15 parts
0.15 part of polyethylene wax serving as a dispersing agent
0.3 part of lubricant zinc stearate
0.15 part of PPA (fluorinated elastomer) as processing aid
However, in the present invention, the preferred composition of the raw material in parts by weight for preparing the above standard sample master batch particles is as in example two, that is, 80 parts of base LDPE resin, 20 parts of calcium carbonate as inorganic opening agent, 0.1 part of 1076 antioxidant, 0.1 part of polyethylene wax as dispersing agent, 0.2 part of zinc stearate as lubricant, and 0.1 part of PPA as processing aid, wherein the density of the standard sample master batch particles prepared from the above raw materials is 1.0547g/cm3The melt mass flow rate MFR was 2.472g/10 min.
The preparation method of the master batch particles of the standard sample of the polyethylene plastic evaporation residues for food packaging adopts the preferable raw material weight parts of the second embodiment to carry out the detailed description of the preparation method, and comprises the following steps:
accurately weighing the raw materials according to the weight parts, pouring 20 parts of inorganic opening agent calcium carbonate, 0.1 part of 1076 antioxidant, 0.1 part of dispersing agent polyethylene wax, 0.2 part of lubricant zinc stearate and 0.1 part of processing aid fluorinated elastomer PPA into a high-speed stirrer, and uniformly mixing with 80 parts of base material LDPE resin; wherein the high-speed stirrer is a Beijing intet GH-50 high-speed stirrer, and is required to be heated to 70 ℃ and to be mixed for 60 minutes at a high speed of 1200 revolutions per minute;
secondly, putting the uniformly mixed materials into a double-screw extruder for melt mixing extrusion, water-cooling and strip-forming in a water tank, then air-drying and cooling, and then drawing the mixture into a granulator for granulation forming to prepare primary sample particles; the double-screw extruder is a ZSK-30 double-screw extruder of Germany WP company, a screw of the double-screw extruder is cleaned by using LDPE resin as a base material before formal feeding, trial feeding is carried out, and formal feeding is carried out after extruded and molded material strips are smooth and free of impurities and no black particles are generated at a grain cutting position; in addition, when the uniformly mixed raw materials are fed into the twin-screw extruder, the temperature of the twin-screw extruder needs to be set as follows: 1 stage 130 ℃; 2, 150 ℃; 3, 160 ℃ in section; 4, 160 ℃ in section; the temperature of the machine head is 150 ℃; the rotating speed of a screw of the double-screw extruder is 230 revolutions per minute, and the diameter of the screw is 30 mm;
thirdly, putting the primary sample particles prepared in the second step into a high-speed stirrer heated to 70 ℃, mixing the primary sample particles at a high speed for 20 minutes at a rotating speed of 1000 revolutions per minute, uniformly mixing the primary sample particles and the high-speed stirrer again, and then sequentially carrying out second melting, mixing, extruding, air-drying, cooling and granulating and forming to prepare secondary sample particles;
fourthly, the secondary sample particles prepared in the third step are put into a high-speed stirrer heated to 70 ℃, are also mixed uniformly at a high speed of 1000 revolutions per minute for 20 minutes, and are subjected to third melting, mixing, extrusion, air drying, cooling and grain-sized forming in sequence to prepare standard sample master batch particles with the particle size of about 2 mm;
fifthly, subpackaging the standard sample master batch particles prepared in the step IV into plastic bags, and drying at room temperature and storing in a sealed manner.
The master batch particles of the standard sample of the polyethylene plastic evaporation residue obtained by the preparation method are dried in a blowing drying hopper for 2 hours at the temperature of 80 ℃ and then are directly injected and molded.
Injection molding:
the preparation of the sample adopts an injection molding mode, a Systec 100-310 type injection molding machine of Sumitomo (SHI) Demag company and an ISO D2 type standard mold of Axico company in the Netherlands are selected, and the injection molding process conditions are as follows:
TABLE 1 injection moulding Process conditions
After the injection molding process conditions are adjusted, injection is started in a full-cycle mode, the first 10 molds are discarded, and a polyethylene plastic evaporation residue standard sample piece is collected from the 11 th mold, wherein the polyethylene plastic evaporation residue standard sample piece is a small square test piece with the size of 60mm in length, 60mm in width and 2mm in thickness.
And (3) testing:
determination of melt mass flow rate:
the melt mass flow rate of the master batch particles of the standard sample of the polyethylene plastic evaporation residues is measured to be 2.472g/10min according to the standard GB/T3682-2000 determination of the melt mass flow rate and the melt volume flow rate of the thermoplastic plastic;
and (3) density measurement:
the density of a sample piece of a standard sample of the polyethylene plastic evaporation residue is measured according to the standard GB/T1033.1-2008' determination of density of non-foamed plastic by part 1 dipping method, hydrometer bottle method and titration method3
Measurement of evaporation residue:
the contact area of a standard sample piece of polyethylene plastic evaporation residue is calculated according to the analysis method of the sanitary standard of polyethylene, polystyrene and polypropylene molded products for food packaging of the Standard GB/T5009.60-2003, and then the calculated contact area is calculated according to 6dm2The contact area corresponds to 1L of soak solution (4% acetic acid), and the migration test is carried out by adopting a complete immersion method, the soaking temperature is 60 ℃, the migration time is 2 hours, and the evaporation residue is 66.0 mg/L.
And (3) testing the uniformity of the standard sample:
randomly extracting 10 parts from prepared standard sample sheets of the polyethylene plastic evaporation residue for uniformity detection, testing the evaporation residue index according to the GB/T5009.60-2003 analytical method for hygienic standards of polyethylene, polystyrene and polypropylene molded products for food packaging, and according to the S <0.3 sigma criterion in GB/T15000.3-2008 standard sample work guide rule (3) standard sample fixed value general principle and statistical method, the sample uniformity evaluation result is shown in the following table:
TABLE 2 homogeneity test data
The verification result shows that the standard deviation of the evaporation residue test data statistics of the prepared sample is less than the critical value of 0.3 sigma =1.35, which indicates that the prepared polyethylene plastic evaporation residue standard sample piece is uniform.
And (3) testing the stability of the standard sample:
stability is another important parameter for measuring standard samples. When the difference between the average values of the two groups of data is considered, the stability of the sample can be evaluated by adopting a 0.3 sigma criterion according to the regulation of GB/T15000.3-2008 'general principle and statistical method for standard sample value determination of standard sample work guide (3)'. The test time interval was 0 month, 6 months, 12 months, 3 samples were randomly taken at each time point, and the assay was performed 2 times in parallel, and the test results are shown in the following table:
table 3 stability test data
The verification results show that the standard deviation of the evaporation residue test data statistics of the prepared sample is less than the critical value of 0.3 sigma =1.35, namely that the prepared polyethylene plastic evaporation residue is not obviously changed, and the prepared standard sample piece is stable within 12 months.
The preparation method of the master batch particles of the standard sample of the evaporation residue in the polyethylene plastic for food packaging solves the problem that the standard sample of the evaporation residue does not exist in the polyethylene plastic industry for food packaging for many years, and provides a powerful technical means for scientific detection and analysis of the content of the evaporation residue in the polyethylene plastic for food packaging.
The above description is only an example of the present invention, and those skilled in the art will understand that any equivalent structure design of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The master batch particles for the standard sample of the polyethylene plastic evaporation residue for food packaging are characterized by comprising the following raw materials in parts by weight:
75-85 parts of base material LDPE resin
19-21 parts of inorganic opening agent calcium carbonate
1076 and 0.05 to 0.15 portion of antioxidant
0.05-0.15 part of dispersing agent polyethylene wax
0.1-0.3 part of lubricant zinc stearate
0.05-0.15 part of PPA (fluorinated elastomer) serving as a processing aid.
2. The polyethylene plastic evaporation residue standard sample master batch particles for food packaging as claimed in claim 1, wherein the density of the standard sample master batch particles is 1.0547g/cm3The melt mass flow rate MFR was 2.472g/10 min.
3. The method for preparing the master batch particles of the standard sample of the polyethylene plastic evaporation residues for food packaging according to claim 1, characterized by comprising the following steps:
accurately weighing the raw materials according to the weight parts, pouring the weighed inorganic opening agent calcium carbonate, 1076 antioxidant, diffusant polyethylene wax, lubricant zinc stearate and processing aid fluorinated elastomer PPA into a high-speed stirrer, and uniformly mixing with the base material LDPE resin;
secondly, putting the uniformly mixed materials into a double-screw extruder for melt mixing extrusion and bracing, performing water-cooling molding through a water tank, then air-drying and cooling, and then drawing the materials into a granulator for granulating molding to obtain primary sample particles;
thirdly, putting the primary sample particles prepared in the second step into a high-speed stirrer for re-mixing, and sequentially carrying out second melting, mixing, extruding, air-drying, cooling, granulating and forming to prepare secondary sample particles;
fourthly, putting the secondary sample particles prepared in the third step into a high-speed stirrer for mixing again, and sequentially carrying out third melting mixing extrusion, air drying cooling and grain cutting molding to prepare standard sample master batch particles;
fifthly, subpackaging the standard sample master batch particles prepared in the step IV into plastic bags, and drying at room temperature and storing in a sealed manner.
4. The preparation method of the master batch particles of the standard sample of the polyethylene plastic evaporation residue for food packaging as claimed in claim 3, wherein in the second step, the screw of the twin-screw extruder is cleaned by using the LDPE resin as the base material, and the master batch is fed after the extruded and molded material strip is smooth and has no impurities and no black particles are produced at the grain cutting position.
5. The method for preparing the master batch particles of the standard sample of the polyethylene plastic evaporation residue for food packaging according to claim 3, wherein in the step (i), a high-speed stirrer for uniformly mixing the raw materials is heated to 70 ℃ and is mixed at a high speed for 60 minutes at a rotating speed of 1200 revolutions per minute; in the third step and the fourth step, the high-speed stirrer is heated to 70 ℃ and is mixed for 20 minutes at a high speed of 1000 revolutions per minute.
6. The method for preparing the master batch particles of the standard sample of the polyethylene plastic evaporation residue for food packaging according to claim 3, wherein in the step II, when the uniformly mixed raw materials are put into a double-screw extruder, the temperature of the double-screw extruder is set as follows: 1 stage 130 ℃; 2, 150 ℃; 3, 160 ℃ in section; 4, 160 ℃ in section; the temperature of the machine head is 150 ℃; the screw rotating speed of the double-screw extruder is 230 r/min, and the screw diameter is 30 mm.
7. The method for preparing the master batch particles of the standard sample of the evaporation residue of the polyethylene plastic for food packaging as claimed in claim 3, wherein the particle size of the master batch particles of the standard sample prepared in the step (iv) is 2 mm.
8. The method for preparing the master batch particles of the standard sample of the evaporation residue of the polyethylene plastic for food packaging as claimed in claim 3, wherein the master batch particles of the standard sample are directly injection molded after being dried in a blowing drying hopper at a temperature of 80 ℃ for 2 hours.
9. The method for preparing the master batch particles of the standard sample of the polyethylene plastic evaporation residues for food packaging according to claim 3, wherein the high-speed stirrer is a Beijing intet GH-50 high-speed stirrer; the twin-screw extruder is a ZSK-30 twin-screw extruder of Germany WP company.
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| CN108276648A (en) | 2018-07-13 |
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