CN102344624B - Preparation method of standard sample for testing phthalic ester plasticizer - Google Patents
Preparation method of standard sample for testing phthalic ester plasticizer Download PDFInfo
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- CN102344624B CN102344624B CN 201110185279 CN201110185279A CN102344624B CN 102344624 B CN102344624 B CN 102344624B CN 201110185279 CN201110185279 CN 201110185279 CN 201110185279 A CN201110185279 A CN 201110185279A CN 102344624 B CN102344624 B CN 102344624B
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- ester plasticizer
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Abstract
The invention provides a preparation method of a standard sample for testing a phthalic ester plasticizer. The preparation method comprises the following steps of: uniformly mixing a phthalic ester plasticizer serving as a target compound with a stabilizer, a lubricant and the like to form a mixture; stirring the mixture and a substrate material at a high speed; stirring, cooling, extruding and blowing to obtain a film of which the thickness is 25-30 mum; and performing serial processing on the film to obtain the standard sample. The invention has the advantages: the standard sample for testing the phthalic ester plasticizer is obtained with the preparation method which is easy and convenient to operate, the comparability and consistence of detection data of the phthalic ester plasticizer in plastic among laboratories are improved, and a basis for uniformly testing the standard of the phthalic ester plasticizer in plastic is laid.
Description
[technical field]
The present invention relates to a kind of preparation method of standard model, relate in particular to a kind of phthalic ester plasticizer and measure the preparation method with standard model.
[background technology]
Phthalic ester plasticizer is mainly used in improving processing characteristics and the intensity of plastics, is widely used in plastics and elastomeric material production.Be connected with Van der Waals force by hydrogen bond between phthalic ester plasticizer and plastic molecules, retain each other relatively independent separately chemical property, phthalic ester plasticizer easily moves in environment from plastics.Scientific research finds that this compounds of phthalic ester plasticizer can disturb human endocrine, the infringement reproduction and development, the states such as European Union, the U.S., Japan formulate the use of such material of regulation limitations in food contact material, toy and youngster's articles for use one after another, as the 2005/84/EC of European Union instruction, 2002/72/EC instruction, U.S.'s consumer's goods improvements in security bills in 2008 etc.Most of toys and articles for children and packaging material for food all contain plastic components, and in plastics, the problem of phthalic ester plasticizer has caused the extensive pass of society.
More about examination criteria and the method for phthalic ester plasticizer in plastics both at home and abroad, examination criteria and method that different testing laboratories adopt are not quite similar.That from the applicant, bears recognizes prison committee's (full name is China national Certification and Accreditation Administration) " mensuration of phthalic ester plasticizer plastics " proficiency testing project in 2009, many laboratory test results differ greatly, through investigating further and analyzing, the plastics phthalic ester plasticizer standard model lacked for test process quality monitoring is an important factor.Therefore, develop as early as possible phthalic ester plasticizer in plastics and measure the detection level for raising food contact material, toy and articles for children manufacturing enterprise and supervision department and social third party laboratory with standard model, guarantee that the aspect tools such as toy and articles for children quality safety are of great significance.
[summary of the invention]
Technical problem to be solved by this invention is to provide a kind of phthalic ester plasticizer to measure the preparation method with standard model, for possibility is laid a good foundation, provided to the unified standard that detects phthalic ester plasticizer in plastics, and simple and convenient, workable characteristics are arranged.
The present invention solves the problems of the technologies described above by the following technical programs: a kind of phthalic ester plasticizer is measured the preparation method with standard model, specifically comprises the steps:
Step 1: the supplementary material of standard specimen is comprised of target compound phthalic ester plasticizer, stablizer, lubricant and body material, according to required appropriate target compound phthalic ester plasticizer and stablizer, the lubricant of taking of standard specimen, and the three is mixed to the formation mixture, and wherein stablizer account for standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight;
Step 2: get body material and mixture described above, and the two is dropped in high speed agitator and is stirred, the speed setting of agitator is 2400 turn/min, and the temperature in agitator stops stirring while rising to 110 ℃～120 ℃ and is cooled to below 45 ℃;
Step 3: the mixture that step 2 is stirred to cooling rear gained is extruded blown film, to produce the film that obtains film thickness 25 μ m～30 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, excise the part of each 20cm of its both sides, the film portion finally remained is standard model again.
Further, phthalic ester plasticizer is measured the preparation method with standard model, it is characterized in that: the condition of extruding blown film in described step 3 is: the rotating speed of blown film motor is 1000～1200 turn/min, and the temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5.
Further, described body material is polyvinyl chloride.
Beneficial effect of the present invention is: by preparation method of the present invention, obtain phthalic ester plasticizer mensuration standard model, contribute to improve between laboratory comparability and consistence that phthalic ester plasticizer in plastics detects data, for possibility is laid a good foundation, provided to the unified standard that detects phthalic ester plasticizer in plastics, to guaranteeing the aspects such as plastic toy and articles for children quality safety, have great importance; In addition, preparation method of the present invention has simple and convenient, workable characteristics.
[embodiment]
Phthalic ester plasticizer of the present invention is measured the preparation method with standard model, the supplementary material that specifically comprises the steps: (1) standard specimen is comprised of target compound phthalic ester plasticizer, stablizer, lubricant and body material, according to required appropriate target compound phthalic ester plasticizer and stablizer, the lubricant of taking of standard specimen, and the three is mixed to the formation mixture, and wherein stablizer account for standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight; (2) get body material and mixture described above, and the two is dropped in high speed agitator and is stirred, the speed setting of agitator is 2400 turn/min, and the temperature in agitator stops stirring while rising to 110 ℃～120 ℃ and is cooled to below 45 ℃; (3) mixture that step 2 is stirred to cooling rear gained is extruded blown film, take to produce and obtain the film that film thickness is 25 μ m～28 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, excise the part of each 20cm of its both sides, the film portion finally remained is standard model again.In addition, in the present invention, comparatively desirable for the film that makes to blow out, the condition of extruding blown film is set as: the rotating speed of blown film motor is 1000～1200 turn/min, and the temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5; Phthalic ester plasticizer can be any one or more in phthalic acid two (2-ethylhexyl) ester (DEHP), dibutyl phthalate (DBP), dinoctyl phthalate (DNOP); Stablizer is organotin, and lubricant is 16～octadecyl alcohol ester and polyene wax; Body material is generally selected has tool under strong representative, normal temperature stability and the material being convenient to deposit preferably in the use, such as polyvinyl chloride (PVC); In plastics, the mensuration of phthalic ester plasticizer content generally adopts solvent extraction, therefore the size of standard model will be guaranteed the consistence of detected result, this to this point, the present invention has made standard model the plastics film of thickness 25 μ m～30 μ m, basic guarantee detected result consistent.
For better the present invention will be described, the present invention is for following several embodiment.
Embodiment mono-
The content of preparation DEHP, DBP, DNOP accounts for respectively the standard model of standard specimen supplementary material gross weight 0.19%, 0.12%, 0.25%:
When the gross weight of standard specimen supplementary material is about 174kg, take respectively 330.6g DEHP, 208.8g DBP, 435gDNOP, 1.74kg organotin and 3.48kg lubricant, and the three is mixed, first said mixture is dropped in high speed agitator, start high speed agitator, drop into polyvinyl chloride (PVC) powder of about 165kg from the top of agitator again, continue to stir, speed setting is 2400 turn/min; Temperature in agitator stops stirring while rising to 110 ℃ and is cooled to below 45 ℃; Adopt inflation film manufacturing machine to be extruded blown film in the mixture that stirs cooling rear gained, the rotating speed of blown film motor is 1100 turn/min, the blown film temperature is 165 ℃, and blow-up ratio is 2.5, produce and obtain the film that film thickness is 28 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, then the part of excising each 20cm of its both sides, the film portion finally remained is standard model.
Embodiment bis-
The content of preparation DEHP, DBP, DNOP accounts for respectively the standard model of standard specimen supplementary material gross weight 0.28%, 0.25%, 0.20%:
When the gross weight of standard specimen supplementary material is about 174kg, take respectively 487.2g DEHP, 435g DBP, 348gDNOP, 2.61kg organotin and 4.35kg lubricant, and the three is mixed, first said mixture is dropped in high speed agitator, start high speed agitator, drop into about 165kg polyvinyl chloride (PVC) powder from the top of high speed agitator again, continue to stir, speed setting is 2400 turn/min; Temperature in agitator stops stirring while rising to 120 ℃ and is cooled to below 45 ℃; Adopt inflation film manufacturing machine to be extruded blown film in the mixture that stirs cooling rear gained, the rotating speed of blown film motor is 1000 turn/min, the blown film temperature is 170 ℃, and blow-up ratio is 2.5, produce and obtain the film that film thickness is 30 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, then the part of excising each 20cm of its both sides, the film portion finally remained is standard model.
Embodiment tri-
The content of preparation DEHP, DBP, DNOP accounts for respectively the standard model of standard specimen supplementary material gross weight 0.28%, 0.25%, 0.20%:
When the gross weight of standard specimen supplementary material is about 174kg, take respectively 487.2g DEHP, 435gDBP, 348gDNOP, 3.48kg organotin and 5.22kg lubricant, and the three is mixed, first said mixture is dropped in high speed agitator, start high speed agitator, drop into about 165kg polyvinyl chloride (PVC) powder from the top of high speed agitator again, continue to stir, speed setting is 2400 turn/min; Temperature in agitator stops stirring while rising to 115 ℃ and is cooled to below 45 ℃; Adopt inflation film manufacturing machine to be extruded blown film in the mixture that stirs cooling rear gained, the rotating speed of blown film motor is 1200 turn/min, the blown film temperature is 160 ℃, and blow-up ratio is 2.5, produce and obtain the film that film thickness is 25 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, then the part of excising each 20cm of its both sides, the film portion finally remained is standard model.
The standard model that the various embodiments described above are obtained is respectively according to GB/T 15000 series standards, adopt GB/T 22048-2008 detection method to carry out uniformity test and stability test, wherein: uniformity test adopts one-factor analysis of variance method (F method), and test show that the F value of made standard model all is less than threshold value F
α(f
1, f
2) (α=0.05 wherein, f
1=14, f
2=30), show that made standard model is uniform; Stability test adopts " mean value consistency check " method in the t method of inspection, and be 10 days, 1 month, 6 months, 12 months the interval time in checkout procedure, and test show that the t value of made standard model all is less than threshold value t
α(n
1+ n
2-2) (α=0.05 wherein, n
1=45, n
2=10), show that made standard model is stable.
To sum up, obtain phthalic ester plasticizer mensuration standard model by preparation method of the present invention, contribute to improve between laboratory comparability and consistence that phthalic ester plasticizer in plastics detects data, laying a good foundation, provide for the unified standard that detects phthalic ester plasticizer in plastics may; In addition, preparation method of the present invention has simple and convenient, workable characteristics.
Claims (3)
1. a phthalic ester plasticizer is measured the preparation method with standard model, and it is characterized in that: it specifically comprises the steps:
Step 1: the supplementary material of standard specimen is comprised of target compound phthalic ester plasticizer, stablizer, lubricant and body material, according to required appropriate target compound phthalic ester plasticizer and stablizer, the lubricant of taking of standard specimen, and the three is mixed to the formation mixture, and wherein stablizer account for standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight; And described phthalic ester plasticizer is any one or more in phthalic acid two (2-ethylhexyl) ester, dibutyl phthalate, dinoctyl phthalate;
Step 2: get body material and mixture described above, and the two is dropped in high speed agitator and is stirred, the speed setting of agitator is 2400 turn/min, and the temperature in agitator stops stirring while rising to 110 ℃～120 ℃ and is cooled to below 45 ℃;
Step 3: the mixture that step 2 is stirred to cooling rear gained is extruded blown film, to produce the film that obtains film thickness 25 μ m～30 μ m, then front 1/5 and rear 1/5 part of this film are given up, only stay the film of middle portion, afterwards after the film rolling of this middle portion, excise the part of each 20cm of its both sides, the film portion finally remained is standard model again.
2. phthalic ester plasticizer as claimed in claim 1 is measured the preparation method with standard model, it is characterized in that: the condition of extruding blown film in described step 3 is: the rotating speed of blown film motor is 1000～1200 turn/min, the temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5.
3. phthalic ester plasticizer as claimed in claim 1 is measured the preparation method with standard model, and it is characterized in that: described body material is polyvinyl chloride.
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| CN 201110185279 CN102344624B (en) | 2011-06-30 | 2011-06-30 | Preparation method of standard sample for testing phthalic ester plasticizer |
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| CN102344624B true CN102344624B (en) | 2013-12-18 |
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| CN105602022B (en) * | 2016-01-29 | 2018-03-23 | 福建出入境检验检疫局检验检疫技术中心 | A kind of preparation method of phenol measure standard rubbers sample |
| CN105647046A (en) * | 2016-04-11 | 2016-06-08 | 北京市理化分析测试中心 | Preparation method of phenolic-antioxidant-containing positive control substance of food contact plastics |
| CN106633505B (en) * | 2016-11-26 | 2021-06-11 | 金发科技股份有限公司 | Preparation method of standard samples of more than ten elements such As As, Se, P and the like in polyvinyl chloride and various phthalates |
| CN106751217B (en) * | 2016-12-28 | 2018-10-26 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN106832881A (en) * | 2017-01-16 | 2017-06-13 | 浙江省计量科学研究院 | Phthalic ester plasticizer and phosphorus flame retardant standard sample and sample preparation methods in polyurethane |
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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 |
| CN108276648B (en) * | 2018-03-13 | 2020-12-15 | 宁波出入境检验检疫局检验检疫技术中心 | Polyethylene plastic evaporation residue standard sample master batch particles for food packaging and preparation method thereof |
| CN112011125B (en) * | 2020-09-07 | 2022-11-11 | 石家庄海关技术中心 | Polypropylene film standard sample with plasticizer migration value and preparation method thereof |
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