CN103645115A - Measurement method for volatile amount of micro-molecular organic matters of plastic additive - Google Patents
Measurement method for volatile amount of micro-molecular organic matters of plastic additive Download PDFInfo
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Abstract
The invention discloses a detection method for the volatile amount of micro-molecular organic matters of a plastic additive. The detection method comprises the following steps: removing water attached to a weighing bottle and treating at 100+/-5 DEG C until the weight is M0; putting a test sample into the weighing bottle with the constant weight and drying at the temperature for 2 hours until the weight is M1; setting different temperatures and heating times according to process requirements of a plastic film and volatilizing the micro-molecular organic matters; after the heating process is finished, metering the weight M2 of the weighing bottle filled with the test sample at a room temperature; and calculating the volatile amount of the micro-molecular organic matters of the test sample according to a computational formula, namely the volatile amount of the micro-molecular organic matters=[(M1-M2)/(M1-M0)]*100%. The micro-molecular volatile amount is less than 0.5% and is used as a control standard when the micro-molecular organic matters as the additive are added into the plastic film. The detection method considers that the additive used in a plastic film production process is strictly selected, has the characteristics of being reliable and high in calculation precision, and is successfully used in a process for producing the high-performance functional film in a plastic processing enterprise.
Description
Technical field
The invention belongs to field of plastics processing, relate in particular to a kind of color concentrate and other adjuvants of plastic processing, the detection method of fluorescence probe volatile quantity under uniform temperature environment.
Background technology
In order to enhance productivity, reduce costs, improve competitiveness, plastic processing enterprise has all adopted raising technological temperature and has increased the technological measures such as additives ratio.Meanwhile, also occurred that product bubble increases, processing equipment die orifice attachment increases needs removing problem frequently, causes product quality to be affected and is restricted with production efficiency.Produce this quality and technological problems, due to general analysis thinks in starting material that moisture content exceeds standard.We,, through after experimental analysis repeatedly, think the problem of plastic additive itself.Because plastic additive is all molecular weight and its strand along with the rising of processing temperature easily fragments into more micromolecular organic material, such as materials such as Tissuemat E, paraffin.These materials can be separated out small organic molecule when high temperature, and its larger molecular organics is with temperature rising molecule chain break, has more increased separating out of small organic molecule.Due to increasing that small organic molecule is separated out, easily there is bubble in product, and processing die orifice attachment increases, and has affected product quality and production work efficiency.
Summary of the invention
In order to solve the problems of the technologies described above, the object of the present invention is to provide a kind of measuring method of plastic additive small organic molecule volatile quantity.
By the detection to plastic additive small molecular organism volatile quantity, emphasis is conceived to the strict selection to additive therefor in plastic foil production technology, so that during plastic foil is produced, under the technological temperature requiring, get rid of the plastic additive that those small organic molecule volatile quantities are high, selection meets the plastic additive of manufacturing technique requirent, can effectively avoid occurring the serious problems such as bubble, processing equipment die orifice attachment increase, and product quality and production efficiency are limited in plastic foil production.
A kind of detection method to plastic additive small organic molecule volatile quantity provided by the invention, comprises the steps:
Step 1: exclude the moisture content that measuring cup adheres to, process to constant weight M0 at the temperature of (100 ± 5) ℃; In the temperature and time of setting, if double baking, put into drying basin, the alleged weight of lowering the temperature is consistent, exclusion volatilization is described, i.e. constant weight.
Step 2, exclude the moisture content in sample to be tested, at the temperature of (100 ± 5) ℃, the measuring cup that sample is housed is processed to constant weight M1;
Step 3, according to plastic foil manufacturing technique requirent, set sample different be subject to temperature and heated time, make its small organic molecule volatilization including, after finished by thermal process, under normal temperature, the weight M2 of the measuring cup of sample is equipped with in metering;
The volatile quantity of the small organic molecule volatilizing in step 4, measuring and calculating sample:
Data M 1, M2 according to measuring, utilize precise weighing method computing formula:
Small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%
In formula, M0 is that Cheng Liang Ping Heng is heavy, and M1 is for getting rid of measuring cup and the sample general assembly (TW) after moisture content, and M2 is under the plastic foil technological temperature time of setting, measuring cup and sample general assembly (TW) that sample small molecular organism is heated and volatilizees,
Calculate the small organic molecule volatile quantity in sample, with little molecule volatile matter < 0.5%, as adjuvant, can be used as the criterion of plastic foil adjuvant.
The object of completing steps one, two is: exempt the interference of moisture content to precise weighing mensuration, get rid of the measuring error that in measuring, moisture content produces, make weighing results more accurate.
In described step 1, exclude measuring cup and adhere to moisture content processing to its constant weight M0, refer to measuring cup is placed in electrically heated drying cabinet, be heated to (100 ± 5) ℃, be incubated 2 hours, in electrically heated drying cabinet, take out, put into the drying basin of drying agent, after naturally near room temperature, with electronic balance, calculate the weight, again measuring cup is put into electric dry oven, continue to dry 0.5 hour, then lower the temperature, then weigh; If double weighing is consistent, illustrate that moisture content dries.This weighing is exactly constant weight M0.
In described step 2, exclude the moisture content in sample to be tested, the measuring cup that sample is housed is processed to constant weight M1, refer to and will be loaded with the measuring cup of sample, insert in the electrically heated drying cabinet of 80-100 ℃, baking 1-3 hour takes out in electrically heated drying cabinet, puts into the drying basin with drying agent, naturally fall and cause after room temperature, the weight of the measuring cup of sample is housed with electronic balance metering; Put into again electrically heated drying cabinet baking 0.5h, then put into drying basin, then lower the temperature, then weigh; If double weighing is consistent, this weight is exactly constant weight M1;
In described step 3 according to plastic foil manufacturing technique requirent, set sample different be subject to temperature and heated time, make its small organic molecule volatilization including, after finished by thermal process, under normal temperature, the weight M2 of the measuring cup of sample is equipped with in metering; Refer to and will get rid of the bottle of weighing of the splendid attire sample of moisture content, insert together heating in electrically heated drying cabinet, when reaching 200-300 ℃, electrothermal drying the temperature inside the box is incubated 0.5-1.5 hour, in electrically heated drying cabinet, take out, naturally fall and cause after room temperature, the weight M2 of the measuring cup of sample is housed with electronic balance metering.
By detection method of the present invention, repeat to do parallel experiment, parallel experiment average error must not surpass 0.5%.
In the present invention, first by baking, remove the moisture content of weighing in bottle, to get rid of moisture content to measuring the error causing; Drying, under dry environment, measure measuring cup and the sample constant weight general assembly (TW) M1 getting rid of after moisture content; Then, according to plastic foil manufacturing technique requirent, by different temperatures, different baking time setting, sample to be tested is heated, its small organic molecule containing is constantly volatilized, when sample to be tested having been completed to the baking temperature of setting, having baked after the time, make it naturally cooling, temperature is down to after room temperature, to the measuring cup of the sample M2 that weighs is housed; By secondary weighing data, can obtain accurately the volatile quantity data of the small organic molecule that plastic additive sample volatilizes in different temperatures, different heated time, data can judge that sampled adjuvant could be as the adjuvant of plastic foil according to this.Thereby solved troubling in the production of plastic functional film and occurred the technical barrier that bubble, processing equipment die orifice attachment increase.
The fidelity factor of detection method of the present invention can reach 100%, has that method is reliable, computational accuracy is high, is successfully used to plastic processing enterprise and manufactures in high performance functional membrane technique.
The present invention is applicable to the test that plastics add material small molecular organism volatile quantity, in the production technologies such as general molded goods, casting films and film goods.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the detection method in the present invention
Embodiment
In the present invention, use instrument, equipment as follows:
Electronic balance, precision 0.1mg; Electrically heated drying cabinet, temperature error is no more than ± and 1 ℃; Flat measuring cup; Drying basin with drying agent.
Metering formula used in the present invention: small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%
Wherein, M0 is measuring cup weight, and M1 is for getting rid of measuring cup and the sample general assembly (TW) after moisture content, and M2 is measuring cup and sample general assembly (TW) after toasting.
Embodiment 1: plastic additive Sample A is at the volatile quantity of 220 ℃ of 1 hour its small organic molecules that is heated
Step 1: remove measuring cup institute water content and make it to constant weight:
Measuring cup is placed in electrically heated drying cabinet, is heated to 100 ℃, be incubated 2 hours, in electrically heated drying cabinet, take out, put into the drying basin of drying agent, after naturally near room temperature, with electronic balance, calculate the weight, then measuring cup is put into electric dry oven, continue to dry 0.5 hour, then lower the temperature, then weigh; If double weighing is consistent, illustrate that moisture content dries.Weigh constant weight M0=11.6340.
Step 2, metering sample to be tested A:
The weight that weighs sample to be tested A with electronic balance is 3g ± 1g;
Moisture content in step 3, eliminating sample to be tested A:
By the sample to be tested A weighing, be placed in the measuring cup M0 processing through constant weight, together with one of vessel, be placed in electrically heated drying cabinet, start electrocaloric effect power supply, electrocaloric effect starts to heat up to Sample A heating in case, when temperature liter causes 95 ℃, be incubated 2 hours, the moisture content containing in sample is volatilized, take out the measuring cup that sample is housed, put into exsiccator, after naturally cooling to room temperature, weigh, if double weighing is consistent, this weight is exactly constant weight M1; With its general assembly (TW) of electronic balance weighing M1=13.8853
;
Step 4
,toast sample to be tested A, measure the volatile quantity of its small organic molecule:
The weight that electronic balance weighing is crossed is the measuring cup that M1 is equipped with described sample, put into electrocaloric effect heating, when rising to 220 ℃, temperature is incubated 1 hour, then make electrocaloric effect naturally cooling, temperature is down to room temperature, the measuring cup of Sample A is equipped with in taking-up, with its general assembly (TW) of electronic balance weighing M2=13.7916;
According to formula: measure Sample A small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%, calculate weight and be the plastic additive Sample A of 3g ± 1g and remove after moisture content, the amount of waving that heats the small organic molecule volatilizing for 1 hour at 220 ℃ is 4.16%.
Embodiment 2 plastic additive sample B are at the volatile quantity of 270 ℃ of 0.5 hour its small organic molecules that is heated
The step of the measuring process of the present embodiment and embodiment 1 is basic identical, and difference is:
Step 1: remove measuring cup institute water content and make it heavy to Heng: this measuring cup constant weight M0 is measured as 12.293;
Moisture content in step 3, eliminating sample to be tested B:
By the sample to be tested B weighing, be placed in the measuring cup M0 processing through constant weight, be placed in electrically heated drying cabinet, start electrocaloric effect power supply, electrocaloric effect starts to heat up to sample B heating in case, when temperature liter causes 80 ℃, is incubated 3 hours, makes the moisture content volatilization containing in sample, after taking-up, put into dry, after near room temperature, weigh, then heat, then cooling weighs, double weighing unanimously, general assembly (TW) M1=14.4167;
Step 4, baking sample to be tested B, measure the volatile quantity of its small organic molecule:
The weight that electronic balance weighing is crossed is the measuring cup that M1 is equipped with described sample, put into electrocaloric effect heating, when rising to 270 ℃, temperature is incubated 0.5 hour, then make electrocaloric effect nature chilling temperature be down to room temperature, the measuring cup of sample B is equipped with in taking-up, with its general assembly (TW) of electronic balance weighing M2=14.3376;
According to formula: measure sample B small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%, calculate weight and be the plastic additive sample B of 3g ± 1g and remove after moisture content, heat 0 at 270 ℃.The amount of waving of the small organic molecule volatilizing for 5 hours is 3.72%.
Embodiment 3 plastic additive sample Chinese wax are at the volatile quantity of 200 ℃ of 1 hour its small organic molecules that is heated
The step of the measuring process of the present embodiment and embodiment 1 is basic identical, and difference is:
Step 1: remove measuring cup institute water content and make it heavy to Heng:
Measuring cup is placed in electrically heated drying cabinet, is heated to 95 ℃, be incubated 2 hours, in electrically heated drying cabinet, take out, put into the drying basin of drying agent, after naturally near room temperature, with electronic balance, calculate the weight, then measuring cup is put into electric dry oven, continue to dry 0.5 hour, then lower the temperature, then weigh; If double weighing is consistent, illustrate that moisture content dries.Weighing constant weight is M0=12.5826;
Moisture content in step 2, eliminating sample Chinese wax:
By the sample Chinese wax weighing, be placed in the measuring cup M0 processing through constant weight, then be placed in electrically heated drying cabinet, start electrocaloric effect power supply, electrocaloric effect starts to heat up to sample Chinese wax heating in case, when causing 95 ℃, temperature liter is incubated 2 hours, make the moisture content volatilization containing in Chinese wax, take out the measuring cup that sample is housed, put into exsiccator, after the near room temperature of temperature, with electronic balance weighing; Put into again electrically heated drying cabinet heating, then lower the temperature, then weigh, if double, weigh consistent, be constant weight, M1=14.8153;
Step 3, baking sample Chinese wax, measure the volatile quantity of its small organic molecule:
The weight that electronic balance weighing is crossed is the measuring cup that M1 is equipped with described sample, put into electrocaloric effect heating, when rising to 200 ℃, temperature is incubated 1 hour, then make electrocaloric effect nature chilling temperature be down to room temperature, the measuring cup of sample Chinese wax is equipped with in taking-up, with its general assembly (TW) of electronic balance weighing M2=14.8091;
According to formula: calculate sample Chinese wax small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%, calculate adjuvant Chinese wax and remove after moisture content, the amount of waving that heats the small organic molecule volatilizing for 1 hour at 200 ℃ is 0.28%.
Embodiment 4 plastic additive sample Chinese wax are at the volatile quantity of 210 ℃ of 1 hour its small organic molecules that is heated
The step of the measuring process of the present embodiment and embodiment 3 is basic identical, and difference is:
Step 1: remove measuring cup institute water content and make it heavy to Heng:
Measuring cup is placed in and in electrically heated drying cabinet, starts heating, be warming up to 100 ℃, be incubated 2 hours, weigh after being placed in the near room temperature of exsiccator, then process to constant weight M0=12.2318;
Moisture content in step 2, eliminating sample Chinese wax:
By the sample Chinese wax weighing, be placed in the measuring cup M0 processing through constant weight, then put into electrically heated drying cabinet, start electrocaloric effect power supply, electrocaloric effect starts to heat up to sample Chinese wax heating in case, when temperature liter causes 95 ℃, is incubated 2 hours, makes the moisture content volatilization containing in Chinese wax, then take out the measuring cup that sample is housed, weigh after being placed in the near room temperature of exsiccator; Put into again electrically heated drying cabinet and heat, then be dried, lower the temperature, be weighed into constant weight, M1=13.8257;
Step 3, baking sample Chinese wax, measure the volatile quantity of its small organic molecule:
The weight that electronic balance weighing is crossed is the measuring cup that M1 is equipped with described sample, put into electrocaloric effect heating, when rising to 210 ℃, temperature is incubated 1 hour, then make electrocaloric effect nature chilling temperature be down to room temperature, the measuring cup of sample Chinese wax is equipped with in taking-up, with its general assembly (TW) of electronic balance weighing M2=13.8165;
According to formula: calculate sample Chinese wax small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%, calculate adjuvant Chinese wax and remove after moisture content, the amount of waving that heats the small organic molecule volatilizing for 1 hour at 210 ℃ is 0.58%.
Embodiment 5
Other step is as embodiment 1, electrothermal drying the temperature inside the box in step 4: 280 ℃, and temperature retention time: 2h.
Table 1
M0: measuring cup weight, M1: for getting rid of measuring cup and the sample general assembly (TW) after moisture content, M2: be measuring cup and the sample general assembly (TW) after baking, little molecule volatile quantity: [(M1-M2)/(M1-M0)] * 100%=4.16% ,/3.72%;
Through twice parallel laboratory test, obtaining micromolecular average volatile quantity is: 3.94%
Embodiment 6
Other step is as embodiment 1, electrothermal drying the temperature inside the box in step 4: 220 ℃, and temperature retention time: 1h
Table 2
Through twice parallel laboratory test, obtain micromolecular average volatile quantity: 3.52%
Embodiment 7
Other step is as embodiment 1, electrothermal drying the temperature inside the box in step 4: 300 ℃, and temperature retention time: 0.5h
Table 3
Through twice parallel laboratory test, obtain micromolecular average volatile quantity: 2.01%
Test one
Test objective: the volatile quantity for starting material when the same time different temperatures is how many, thus judge in concrete blown film production process and under required blown film time-temperature condition, whether select this material to add raw material as producing.
Take Chinese wax as test material, and other step is as embodiment 1, and one hour heat time in step 4, while recording different temperatures, little molecule thing volatile quantity data are as table 4:
The little molecule volatile matter of table 4 different temperatures volatile quantity test figure table
The little molecule thing volatile quantity of sample is [(M1-M2)/(M1-M0)] * 100%.
From upper table 4, within the identical heat time, Chinese wax small organic molecule volatile quantity progressively rises with heating-up temperature rising volatile quantity.But when heating-up temperature is increased to volatilization temperature (being 245 ℃ of left and right), volatile quantity sharply rises.Can determine thus that in film-blowing process process blown film temperature is that can not select Chinese wax when more than 210 ℃ be raw materials for production, selects other raw material to produce, to obtain the good plastic products of quality thus.
Test two
Test objective: the volatile quantity for starting material when the uniform temp different time is how many, thus judge in concrete blown film production process and under required blown film time-temperature condition, whether select this material as producing adjuvant.
Material, the same test one of equipment, other step is as embodiment 1, electrothermal drying the temperature inside the box in step 4: 220 ℃.
Test figure is as following table 5:
The little molecule thing of table 5 temporal evolution volatile quantity testing record sheet
From upper table 5, under certain heating-up temperature, the little molecule volatile matter of sample increased with the heat time.Can determine thus in the film-blowing process process blown film temperature one regularly, the time be 50min can not select Chinese wax when above be production adjuvant, select thus other adjuvant to produce, to obtain the good plastic products of quality.
Test three
Test objective: by identical raw material, identical mass parts, 1,2,3,4,5,6 groups of the masterbatch made from different little molecule volatile quantity raw materials, under identical material, process conditions, be blow molded into the film of same thickness, appoint and get one square metre of its bubble of product meter, pin hole, amount of speckle.
Film blowing device: individual layer inflation film manufacturing machine; Error range ± 5 ℃. thickness 2 μ.
Test figure is as following table 6:
Table 6
Conclusion: from above table 6, during little molecule volatile matter < 0.5% in masterbatch, blown film can not produce obvious bubble, pin hole, spot, after > 0.5%, little molecule volatile matter increases, the bubble producing, pin hole, spot increase, and therefore, it is the index of economical rationality that the present invention gets little molecule volatile matter < 0.5%.
Claims (4)
1. a detection method for plastic additive small organic molecule volatile quantity, comprises the steps:
Step 1, exclude the moisture content that measuring cup adheres to, at 95-105 ℃ of temperature, process to constant weight M0;
Step 2, exclude the moisture content in sample to be tested, in the measuring cup to constant weight, pack sample into, at the temperature of 95-105 ℃, the measuring cup that sample is housed is processed to constant weight M1;
Step 3, according to plastic foil manufacturing technique requirent, set different heating temperature and the heated times of sample, make its small organic molecule volatilization including, after finished by thermal process, under normal temperature, the weight M2 of the measuring cup of sample is equipped with in metering;
The volatile quantity of the small organic molecule volatilizing in step 4, calculating sample:
Data M 1, M2 according to measuring, utilize precise weighing method computing formula:
Small organic molecule volatile quantity=[(M1-M2)/(M1-M0)] * 100%
In formula, M0 is that Cheng Liang Ping Heng is heavy, and M1 is for getting rid of measuring cup and the sample general assembly (TW) after moisture content, and M2 is at the plastic foil technological temperature of setting, under the time, measuring cup and sample general assembly (TW) after the volatilization of sample small molecular organism,
Calculate the small organic molecule volatile quantity in sample, with the little molecule volatile quantity of sample < 0.5%, as adjuvant, can be used as the criterion that plastic foil adds.
2. the detection method of plastic additive small organic molecule volatile quantity according to claim 1, is characterized in that:
In described step 1: exclude measuring cup and adhere to moisture content processing to its constant weight M0, refer to measuring cup is placed in electrically heated drying cabinet, be heated to 95-105 ℃, be incubated 2 hours, in electrically heated drying cabinet, take out, put into the drying basin of drying agent, be naturally down to after room temperature, with electronic balance, calculate the weight; Again measuring cup is put into electric dry oven, continue to dry 0.5 hour, then lower the temperature, then weigh; If double weighing is consistent, illustrate that moisture content dries, this weighing is exactly constant weight M0.
3. the detection method to plastic additive small organic molecule volatile quantity according to claim 1, it is characterized in that: in described step 2: exclude the moisture content in sample to be tested, the measuring cup that sample is housed is processed to constant weight M1, refer to and will be loaded with the measuring cup of sample, insert in the electrically heated drying cabinet of 80-100 ℃, baking 1-3 hour, in electrically heated drying cabinet, take out, put into the drying basin with drying agent, naturally fall and cause after room temperature, the weight of the measuring cup of sample is housed with electronic balance metering; If double weighing is consistent, this weight is exactly constant weight M1.
4. the detection method of plastic additive small organic molecule volatile quantity according to claim 1, it is characterized in that: in described step 3: according to plastic foil manufacturing technique requirent, set different heating temperature and the heated times of sample, the small organic molecule volatilization that it is included, after finished by thermal process, under normal temperature, the weight M2 of the measuring cup of sample is equipped with in metering; Refer to and will get rid of the bottle of weighing of the splendid attire sample of moisture content, insert together heating in electrically heated drying cabinet, when electrothermal drying the temperature inside the box reaches 200-300 ℃, insulation 0.5-1.5 hour, in electrically heated drying cabinet, take out, naturally be down to after room temperature, the weight M2 of the measuring cup of sample is housed with electronic balance metering.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103926166A (en) * | 2014-04-25 | 2014-07-16 | 上海市机械制造工艺研究所有限公司 | Method for detecting solvent volatilization rate in V-method casting coating |
| CN105510172A (en) * | 2015-12-15 | 2016-04-20 | 上海宝钢磁业有限公司 | Measuring method for content of polyvinyl alcohol in manganese zinc ferrite material powder |
| CN108204932A (en) * | 2016-12-19 | 2018-06-26 | 内蒙古蒙牛乳业（集团）股份有限公司 | The method for detecting volatile content in grease |
| CN109580414A (en) * | 2018-10-19 | 2019-04-05 | 江苏浦金药业有限公司 | A kind of method of inspection of Venenum Bufonis Injection |
| CN110196203A (en) * | 2019-05-13 | 2019-09-03 | 深圳市家具行业协会 | A kind of adhesive or water content of coating and total volatile organism content quick determination method |
| CN111307649A (en) * | 2020-03-12 | 2020-06-19 | 北京市环境保护科学研究院 | Method for detecting content of volatile organic compounds in asphalt |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926166A (en) * | 2014-04-25 | 2014-07-16 | 上海市机械制造工艺研究所有限公司 | Method for detecting solvent volatilization rate in V-method casting coating |
| CN105510172A (en) * | 2015-12-15 | 2016-04-20 | 上海宝钢磁业有限公司 | Measuring method for content of polyvinyl alcohol in manganese zinc ferrite material powder |
| CN108204932A (en) * | 2016-12-19 | 2018-06-26 | 内蒙古蒙牛乳业（集团）股份有限公司 | The method for detecting volatile content in grease |
| CN109580414A (en) * | 2018-10-19 | 2019-04-05 | 江苏浦金药业有限公司 | A kind of method of inspection of Venenum Bufonis Injection |
| CN110196203A (en) * | 2019-05-13 | 2019-09-03 | 深圳市家具行业协会 | A kind of adhesive or water content of coating and total volatile organism content quick determination method |
| CN111307649A (en) * | 2020-03-12 | 2020-06-19 | 北京市环境保护科学研究院 | Method for detecting content of volatile organic compounds in asphalt |
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Application publication date: 20140319 |