CN105136611B - A kind of tacky performance fast appraisement method of butyl rubber plug - Google Patents
A kind of tacky performance fast appraisement method of butyl rubber plug Download PDFInfo
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- CN105136611B CN105136611B CN201510583384.9A CN201510583384A CN105136611B CN 105136611 B CN105136611 B CN 105136611B CN 201510583384 A CN201510583384 A CN 201510583384A CN 105136611 B CN105136611 B CN 105136611B
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Abstract
The present invention relates to a kind of tacky performance fast appraisement method of butyl rubber plug, it is specially：Pre-treatment is carried out to butyl rubber plug with 0.3%NaOH solution, butyl rubber plug is taken, and check plug sample size N, it is placed in plastic-aluminum combined film packaging bag, gently shaking makes plug try one's best after close concentrate, and carries out vacuumizing heat seal, evacuated pressure 0.09Mpa on vacuum packing machine.Butyl rubber plug after encapsulation is placed in constant temperature and humidity incubator, design temperature is 65 DEG C, and humidity is 70%.Packaging bag is taken out after 5 days, it is cooled to normal temperature, the bag observation tacky situation of plug is opened, the tacky level of butyl rubber plug is evaluated by opening butyl rubber plug conglomeration individual amount S after bag 4h, and define conglomeration individual to open some butyl rubber plugs for being not affected by external force factor influence after bag and bonding together naturally.The present invention is quantified to evaluation result, and proposes specific decision method, and the tacky performance of butyl rubber plug fast and effectively can be evaluated.
Description
Technical field
The present invention relates to a kind of tacky performance fast appraisement method of butyl rubber plug, belong to field of rubber materials.
Background technology
Current drug safety turns into the great society problem that the whole people pay close attention to, and butyl rubber plug (hereinafter referred to as plug) is as direct
A class Medical Packing Materials of medicine are contacted, its quality directly affects drug quality, closely bound up with whole people's drug safety.
When pharmaceutical production producer uses plug, often occur that plug is inter-adhesive, conglomeration after sterilizing cooling, cause plug not
Can it is smooth walk machine, to pharmaceutical factory production make troubles, while influence drug quality.This phenomenon is referred to as the tacky phenomenon of plug by us.
Cause that the reason for plug is tacky has formula design defect, plug structure design defect, production technology fluctuation, pharmaceutical factory is improper uses
Deng.Therefore during plug new-product development stage, technique adjustment, production equipment debugging after etc. multiple periods need to plug
Tacky performance is evaluated, and has ensured plug product quality.But the current evaluation for the tacky performance of plug is without unified mark
It is accurate.Some Enterprises, which are taken, to carry out plug vanning to observe tacky situation after heavy burden is stacked for a long time, but the method usually requires 30
My god, evaluate timeliness low, it is impossible to which Fast Evaluation is made to the tacky performance of plug.Also by be affectedly bashful plug vulcanization after feel and resilience
Property anticipation is carried out to the tacky performance of plug, although the method timeliness is fast, accuracy is not high, and tacky index can not be measured
Change.
The content of the invention
It is an object of the invention to provide a kind of tacky performance fast appraisement method of butyl rubber plug, harsh experiment condition is utilized
The tacky process of plug is quickly effectively simulated, and the tacky performance of plug quantified using conglomeration individual amount S, to evaluating fourth
The tacky performance of base rubber plug is provided with beneficial guidance.
Technical scheme：A kind of tacky performance fast appraisement method of butyl rubber plug.Plug surface is in vulcanization and clearly
Two production processes meeting adhesion section silicone oil are washed, the silicone oil amount on plug surface can directly affect the correct of the tacky degree of plug and sentence
It is fixed, therefore pre-treatment removal plug surface silicone oil need to be carried out to plug, it is ensured that plug surface siliconization state consistency.High temperature and high pressure
Harsh experiment condition can accelerate the adhesion process between plug, but temperature and pressure sets and too high all plugs can be caused to go out
Existing adhesion phenomenon, it is impossible to draw correct result of determination, temperature and pressure that the present invention has verified preferred suitably by long-term experiment
Power, establishes the tacky process of speeding-up simulation plug under harsh experiment condition.Integrated by butyl rubber plug conglomeration individual amount S
Evaluate the tacky level of butyl rubber plug.If S values are lower, show that plug is tacky more serious, on the contrary it is slighter.The present invention can be quickly effective
The tacky situation of plug is simulated, and its tacky degree can be quantified, and it is fast to this by experimental method of bearing a heavy burden for a long time
Fast evaluation method is verified, it was demonstrated that the validity of the fast appraisement method result.Specific experiment method is as follows：
A, plug pre-treatment：Plug is submerged using 0.3%NaOH solution, is placed in high-pressure sterilizing pot, 121 DEG C of processing
30min.Take the dish out of the pot after cooling, discard alkali lye and rinsed three times using purified water, be subsequently placed in 0.1%HCl solution and soak 10min,
Discard acid solution using purified water rinse three times, plug is transferred in stainless steel disc, be placed in 105 DEG C of baking ovens plug is dried it is stand-by.
The tacky process speeding-up simulation of b, plug：After pre-treatment, butyl rubber plug (particular number and the plug specification of corresponding amount are taken
It is shown in Table 1), and checks plug sample size N, is placed in thickness for 0.125mm, long 360mm, width 270mm plastic-aluminum combined film packaging
In bag, gently shaking makes plug try one's best after close concentrate, and carries out vacuumizing heat seal, evacuated pressure on vacuum packing machine
0.09Mpa, heat seal linear distance plug 2cm, heat seal width are 1cm, and (heat seal parameter is with optimal heat seal by heat sealed time 5s
Intensity is standard).Butyl rubber plug after encapsulation is placed in constant temperature and humidity incubator, design temperature is 65 DEG C, and humidity is 70%.
Every bag of sample message is identified in detail before being put into incubator, and records the cartonning time.Packaging bag is taken out after 5 days, is cooled down
To normal temperature, the bag observation tacky situation of plug is opened.
The plug specification of table 1 and correspondence sample size
| Numbering | Plug specification | Sample size/only |
| 1 | The liquid drugs injections of Φ 13 | 1500 |
| 2 | Φ 13 is freezed | 1000 |
| 3 | The powder pins of Φ 20 | 500 |
| 4 | Φ 20 is freezed | 400 |
| 5 | Φ 26 infuses | 250 |
| 6 | Φ 28 infuses | 200 |
| 7 | Φ 32 infuses | 100 |
C, conglomeration individual S are defined：Open some butyl rubbers that external force factor influence is not affected by after bag and is bonded together naturally
Plug, wherein monobutyl plug are also calculated as conglomeration individual.
D, conglomeration individual amount S determination：Open the package after 4h, check conglomeration individual amount, open bag and check process
Holding is handled with care, and the influence of external force is reduced as far as possible.
E, tacky performance result judgement：The tacky level of plug is judged according to S and plug sample size N ratio, if S >=
60%N then judges that tacky performance is qualified；Also contrasting detection can be carried out with the qualified sample of known tacky performance, S values are more than contrast
Sample keeps same level with control sample, and it is qualified to be determined as.When several same specification samples contrast preferred, then S values are bigger, tackiness
Can be more excellent.
F, long-term bear a heavy burden stack experimental verification：It is real that the confirmatory experiment need to carry out contrast with the plug sample of known tacky degree
Test.Carry out after pre-treatment, take the butyl rubber plug (particular number and plug specification are shown in Table 2) of corresponding amount, be placed in long 650mm, width
450mm polyethylene aseptic package bag carries out double-deck encapsulation, and each laboratory sample encapsulates two bags, by two bags of packaged plugs
It is placed in long 440mm, width 350mm, high 210mm corrugated case and carries out sealing packing.Placed under uniform heavy burden 60kg, normal temperature condition
The bag observation tacky situation of plug is opened after 30 days.When being opened bag by observation after plug adhesion state, shaking plug situation of being scattered, it is right
Than the tacky degree for analyzing plug.
The plug specification of table 2 and correspondence every bag of plug encapsulation amount of sample
| Numbering | Plug specification | Every bag of plug encapsulation amount/only |
| 1 | The liquid drugs injections of Φ 13 | 15000 |
| 2 | Φ 13 is freezed | 10000 |
| 3 | The powder pins of Φ 20 | 5000 |
| 4 | Φ 20 is freezed | 3500 |
| 5 | Φ 26 infuses | 2500 |
| 6 | Φ 28 infuses | 1800 |
| 7 | Φ 32 infuses | 800 |
The invention has the advantages that：
1st, the method that the present invention proposes a kind of tacky performance evaluation of plug, unification is established for the examination tacky performance of plug
Normative reference, can promote plug quality level lifted.
2nd, method provided by the present invention can be evaluated quickly the tacky performance of plug.
3rd, the present invention more convenient can be evaluated the tacky performance of plug exactly.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
The A formula injection sterile powders chlorinated butyl rubber bung (production that different sulfuration process are produced using the present invention
Product specification is the powder pins of Φ 20), the Fast Evaluation of tacky performance is carried out, and experiment progress is stacked by bearing a heavy burden for a long time checking checking.
The specific difference of sample is shown in Table 3.
The sample message table of table 3
| Sample number into spectrum | Formula | Curing temperature | Cure time |
| 1 | A | 165℃ | 240 |
| 2 | A | 170℃ | 240 |
| 3 | A | 175℃ | 240 |
| 4 | A | 180℃ | 240 |
Fast appraisement method：
4 kinds of sample plugs and comparative sample plug are submerged respectively using 0.3%NaOH is molten, mark is placed in high pressure after distinguishing
In autoclave, 121 DEG C of processing 30min.Take the dish out of the pot after cooling, discard alkali lye and rinsed three times using purified water, be subsequently placed in 0.1%
10min is soaked in HCl solution, acid solution is discarded and is rinsed three times using purified water, plug is transferred in stainless steel disc, 105 DEG C are placed in
Baking oven dries plug stand-by.
4 kinds of samples of accurate counting and each 500 of comparative sample, it is 0.125mm, long 360mm, width 270mm to be placed in thickness
In plastic-aluminum combined film packaging bag, gently shaking makes plug try one's best after close concentrate, and carries out vacuumizing heat on vacuum packing machine
Sealing, evacuated pressure 0.09Mpa, heat seal linear distance plug 2cm are closed, heat seal width is 1cm, heat sealed time 10s.
Butyl rubber plug after encapsulation is placed in constant temperature and humidity incubator, design temperature is 65 DEG C, and humidity is 70%.Be put into incubator it
It is preceding that every bag of sample message is identified in detail, and record the cartonning time.Packaging bag is taken out after 5 days, normal temperature is cooled to, bag sight is opened
Examine the tacky situation of plug.Specific visual observation is shown in Table 4.
The conglomeration individual amount S of the various samples of table 4
Judged according to experimental result, the tacky performance of sample 3#, 4# is qualified, and thus judge that 3# sample sulfuration process is reasonable.
Long-term bear a heavy burden stacks experiment：
4 kinds of samples of accurate counting and each 5000 of comparative sample, are placed in long 650mm, width 450mm polyethylene aseptic packaging
Bag carries out double-deck encapsulation, and each laboratory sample encapsulates two bags, two bags of packaged plugs are placed in into long 440mm, width 350mm, height
210mm corrugated case carries out sealing packing.Bag observation plug is opened after being placed 30 days under uniform heavy burden 60kg, normal temperature condition tacky
Situation.Observation result show, the serious adhesion of 1# products, and plug is adhesive into one when opening bag, is shaken and is not dissipated；2# products slightly glue
Even, plug is adhesive into one when opening bag, and part plug is scattered after shaking；Plug does not glue loosely when comparative sample and 3#, 4# are opened bag
Even.
Long-term stacking experiment results of bearing a heavy burden are consistent with the inventive method evaluation result.
Claims (5)
1. a kind of tacky performance fast appraisement method of butyl rubber plug, it is characterised in that specific evaluation procedure is as follows：
A, plug pre-treatment：Plug is submerged using NaOH solution, is placed in high-pressure sterilizing pot, 121 DEG C of processing 30min take the dish out of the pot
After cooling, discard alkali lye and rinsed three times using purified water, be subsequently placed in HCl solution and soak 10min, discard acid solution and use purifying
Water rinse three times, plug is transferred in stainless steel disc, be placed in 105 DEG C of baking ovens plug is dried it is stand-by；
The tacky process speeding-up simulation of b, plug：The butyl rubber plug of corresponding amount is taken, and checks plug sample size N, is placed in plastic-aluminum combined
In film packaging bag, gently shaking makes plug try one's best after close concentrate, and carries out vacuumizing heat seal on vacuum packing machine, takes out
Vacuum pressure 0.09Mpa, heat seal linear distance plug 2cm, heat seal width are 1cm, heat sealed time 5s, after encapsulation
Butyl rubber plug is placed in constant temperature and humidity incubator, and design temperature is 65 DEG C, and humidity is 70%, is put into before incubator to every bag of sample
Product information is identified in detail, and takes out packaging bag after recording cartonning time, 5 days, is cooled to normal temperature, opens bag observation plug tacky
Situation；
C, conglomeration individual amount S determination：Open the package after 4h, check conglomeration individual amount, open bag and check process holding
Handle with care, the influence of external force is reduced as far as possible；
D, tacky performance result judgement：The tacky level of plug is judged according to S and plug sample size N ratio, if S >=60%N
Judge that tacky performance is qualified；When several same specification samples contrast preferred, then S values are bigger, and tacky performance is more excellent.
2. the tacky performance fast appraisement method of butyl rubber plug according to claim 1, it is characterised in that NaOH in step a
Solution is the NaOH solution that mass concentration is 0.3%；HCl solution is the HCl solution that mass concentration is 0.1%.
3. the tacky performance fast appraisement method of butyl rubber plug according to claim 1, it is characterised in that plastic-aluminum in step b
The thickness of Laminated plastic film package bag is 0.125mm, long 360mm, width 270mm.
4. the tacky performance fast appraisement method of butyl rubber plug according to claim 1, it is characterised in that in step c, conglomeration
Individual is opens some butyl rubber plugs that external force factor influence is not affected by after bag and is bonded together naturally, wherein single butyl rubber plug
Also it is calculated as conglomeration individual.
5. a kind of tacky performance fast appraisement method of butyl rubber plug, it is characterised in that specific evaluation procedure is as follows：
A, plug pre-treatment：Plug is submerged using NaOH solution, is placed in high-pressure sterilizing pot, 121 DEG C of processing 30min take the dish out of the pot
After cooling, discard alkali lye and rinsed three times using purified water, be subsequently placed in HCl solution and soak 10min, discard acid solution and use purifying
Water rinse three times, plug is transferred in stainless steel disc, be placed in 105 DEG C of baking ovens plug is dried it is stand-by；
The tacky process speeding-up simulation of b, plug：The butyl rubber plug of corresponding amount is taken, and checks plug sample size N, is placed in plastic-aluminum combined
In film packaging bag, gently shaking makes plug try one's best after close concentrate, and carries out vacuumizing heat seal on vacuum packing machine, takes out
Vacuum pressure 0.09Mpa, heat seal linear distance plug 2cm, heat seal width are 1cm, heat sealed time 5s, after encapsulation
Butyl rubber plug is placed in constant temperature and humidity incubator, and design temperature is 65 DEG C, and humidity is 70%, is put into before incubator to every bag of sample
Product information is identified in detail, and takes out packaging bag after recording cartonning time, 5 days, is cooled to normal temperature, opens bag observation plug tacky
Situation；
C, conglomeration individual amount S determination：Open the package after 4h, check conglomeration individual amount, open bag and check process holding
Handle with care, the influence of external force is reduced as far as possible；
D, tacky performance result judgement：An individual amount S and known tacky performance qualified sample is subjected to contrasting detection, S
Value keeps same level more than control sample or with control sample, and it is qualified to be determined as.
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| CN201510583384.9A CN105136611B (en) | 2015-09-15 | 2015-09-15 | A kind of tacky performance fast appraisement method of butyl rubber plug |
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| CN105136611B true CN105136611B (en) | 2017-09-22 |
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Address after: No. 499, Donglin Road, biological industry park, Yichang District, China (Hubei) free trade zone, Yichang City, Hubei Province Patentee after: Hubei Huaqiang Technology Co., Ltd Address before: 443003 Hubei province Yichang City Kiln Road No. 45 Patentee before: HUBEI HUAQIANG HIGH-TECH Co.,Ltd. |
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