CN108020481A - A kind of test method of swell rubber degree - Google Patents

A kind of test method of swell rubber degree Download PDF

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Publication number
CN108020481A
CN108020481A CN201711263286.2A CN201711263286A CN108020481A CN 108020481 A CN108020481 A CN 108020481A CN 201711263286 A CN201711263286 A CN 201711263286A CN 108020481 A CN108020481 A CN 108020481A
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CN
China
Prior art keywords
sample
test method
degree
quality
swell rubber
Prior art date
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Pending
Application number
CN201711263286.2A
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Chinese (zh)
Inventor
曹祥薇
杨光远
韩磊
周向东
王明慧
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WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT Co Ltd
Original Assignee
WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT Co Ltd
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Application filed by WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT Co Ltd filed Critical WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT Co Ltd
Priority to CN201711263286.2A priority Critical patent/CN108020481A/en
Publication of CN108020481A publication Critical patent/CN108020481A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/02Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content

Abstract

A kind of test method of swell rubber degree of the present invention, comprises the following steps:(1), measure the quality of sample;(2), will weigh after the sample be swollen under water-bath using solvent;(3), since the swelling every 20~24h measurements once sample quality, until the difference of adjacent measured value twice is 0.01g~0.005g, writing down the measured value is

Description

A kind of test method of swell rubber degree
Technical field
The present invention relates to rubber processing techniques field, more particularly to a kind of test method of swell rubber degree.
Background technology
The key of evaluation crosslinked polymer degree is to measure the degree of cross linking of cross-linked polymer.Currently, cross-linked polymer is measured The means of the degree of cross linking mainly have extraction, infrared method, thermal deformation method and hot extension method.Infrared method is higher to equipment requirement, generally Laboratory will not be equipped with.The extractant of the degree of cross linking of extraction measure cross-linked polymer is usually dimethylbenzene single solvent, however, It is relatively low using the extraction efficiency of the extractant.High molecular dissolving is a relatively slow process, can be divided into swelling and dissolving Two stages, swelling refer to that solvent molecule is diffused into inside macromolecule, make the phenomenon of its volumetric expansion.Swelling is macromolecule material Expect distinctive phenomenon, its reason is that solvent molecule differs greatly with coil dimension, and molecular motion velocities differ greatly, solvent Molecular diffusion rates are very fast, and diffusion of the macromolecule into solvent is slow.Therefore, it is that solvent molecule oozes first during macromolecule dissolution Penetrate into inside high molecular material, increase its volume, that is, be swollen.Continuous with solvent molecule is penetrated into, the macromolecule of swelling Material volume constantly increases, macromolecular chain segment movement enhancing, then reaches whole macromolecular chain by the coordinated movement of various economic factors of segment Movement, macromolecular are progressed into solution, form thermodynamically stable homogeneous system, i.e. dissolution phase.
Because crosslinking is to improve a kind of size of very important method degrees of cross linking and the property of rubber of rubber performance Can be directly related, therefore when being processed to rubber, control conditions of vulcanization, keep the appropriate degree of cross linking just to become actual processing During crucial step.The relation of rubber cross degree to be understood and product properties, must just measure the swellbility of rubber.
In the prior art, the measure of swellbility is relatively complicated, and measuring accuracy is relatively low.
The content of the invention
It is an object of the present invention to for the above-mentioned deficiency of the prior art, propose that a kind of step is simple, testing result is opposite A kind of accurate test method of swell rubber degree.
A kind of test method of swell rubber degree of the present invention, comprises the following steps:
(1), measure the quality Q UOTE of sample
(2), will weigh after the sample be swollen under water-bath using solvent;
(3), since the swelling every 20~24h measurements once sample quality, until adjacent measurement twice The difference of value is 0.01g~0.005g, and it is QUOTE to write down the measured value
Preferably, the solvent be essential oil 2630, Peppermint essential oil, one kind in coffee essential oil or at least two kinds.
Preferably, the temperature range of the water-bath is 5~100 DEG C.
Preferably, the temperature range of the water-bath is 20 DEG C~25 DEG C.
Preferably, using a ten thousandth balance measurement sample quality.
Preferably, step(3)In every time take out sample after, rapidly with filter paper blot sample surfaces adhere to solvent, immediately It is put into measuring cup, weighs after covering tightly bottle stopper, then puts again in swelling pipe and continue to be swollen.
Preferably, the quality Q UOTE of the sample Scope be 0.3~0.5g.
Preferably, step(1)Also include first empty measuring cup being weighed on a ten thousandth balance, then toward putting in measuring cup Enter-block sample, be re-weighed, obtain the quality Q UOTE of sample
The method that swell rubber degree is tested in the present invention, by the sample to be tested immersion of certain mass in a solvent, by every Every regular time, a sample quality is measured, draw swellbility by the front and rear mass change of calculating swelling hands over to characterize Connection degree, method of the invention is easy to operate, safe and non-toxic, and the test method of the present invention is applied in the process of rubber, By controlling conditions of vulcanization, keeping the appropriate degree of cross linking, rubber performance is effectively improved.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is further described, but the present invention is simultaneously It is not limited to these embodiments.
Embodiment 1
Rubber of the degree of cross linking less than 80% is taken to be swollen in essential oil 2630, the test method of swell rubber degree, comprises the following steps:
(1), on a ten thousandth balance first empty measuring cup is weighed, then toward-block sample is put into measuring cup, be re-weighed, ask Go out the quality Q UOTE of sample ;(2), the sample after weighing is put into Boiling tube, add 2630 essential oil (quantity of solvent About at test tube l/3), cover tightly test tube plug and then test tube is put into water bath with thermostatic control and be swollen.
(3),-secondary sample quality is measured every the 24h times later, lightly to take out swelling body every time rapidly with filter Paper blots the solvent of sample surfaces attachment, is immediately placed in measuring cup, weighs after covering tightly bottle stopper, then puts in swelling pipe and continues again Swelling.Until the difference of quality weighed up twice is no more than 0.01g, that is, think that swelling process reaches balance, the matter after swelling equilibrium Amount is denoted as QUOTE
(4), calculate the front and rear mass change QUOTE of sample swelling , QUOTE .Specific experiment conclusion is shown in Table 1.
(5), analysis:From 24h in table 1 48h 72h experimental result, rubber sample is swollen flat in 2630 solution Within 1% this minor variations can be neglected, it is believed that the sample is in 2630 essential oils substantially without swelling in mass change after weighing apparatus.
Embodiment 2
Rubber of the degree of cross linking less than 80% is taken to be swollen in essential oil peppermint, the test method of swell rubber degree, comprises the following steps:
(1), on a ten thousandth balance first empty measuring cup is weighed, then toward-block sample is put into measuring cup, be re-weighed, ask Go out the quality Q UOTE of sample
(2), the sample after weighing is put into Boiling tube, add Peppermint essential oil (quantity of solvent is about located to test tube l/3), cover Then test tube is put into water bath with thermostatic control by tight test tube plug is swollen.
(3),-secondary sample quality is measured every the 24h times later, lightly to take out swelling body every time rapidly with filter Paper blots the solvent of sample surfaces attachment, is immediately placed in measuring cup, weighs after covering tightly bottle stopper, then puts in swelling pipe and continues again Swelling.Until the difference of quality weighed up twice is no more than 0.01g, that is, think that swelling process reaches balance, the matter after swelling equilibrium Amount is denoted as QUOTE
(4), calculate the front and rear mass change QUOTE of sample swelling , QUOTE .Specific experiment conclusion is shown in Table 2.
(5), analysis:From 24h in table 2 48h 72h experimental result, rubber sample is swollen flat in 2630 solution Within 1% this minor variations can be neglected, it is believed that the sample is in Peppermint essential oil substantially without swelling in mass change after weighing apparatus.
Embodiment 3
Rubber of the degree of cross linking less than 80% is taken to be swollen in essential oil peppermint, the test method of swell rubber degree, comprises the following steps:
(1), on a ten thousandth balance first empty measuring cup is weighed, then toward-block sample is put into measuring cup, be re-weighed, ask Go out the quality Q UOTE of sample
(2), the sample after weighing is put into Boiling tube, add Peppermint essential oil (quantity of solvent is about located to test tube l/3), cover Then test tube is put into water bath with thermostatic control by tight test tube plug is swollen.
(3),-secondary sample quality is measured every the 24h times later, lightly to take out swelling body every time and use rapidly Filter paper blots the solvent of sample surfaces attachment, is immediately placed in measuring cup, weighs after covering tightly bottle stopper, then puts swelling pipe relaying again Continuous swelling.Until the difference of quality weighed up twice is no more than 0.01g, that is, think that swelling process reaches balance, after swelling equilibrium Quality is denoted as QUOTE
(4), calculate the front and rear mass change QUOTE of sample swelling , QUOTE .Specific experiment conclusion is shown in Table 3.
(5), analysis:From 24h in table 3 48h 72h experimental result, rubber sample is in coffee essence oil solution Mass change is in the ascendant trend of 2%/24h, illustrates that sample has Swelling in coffee essence oil solution.
Table 1
Table 1
Table 1
Contrast three embodiments, it can be seen that there is some difference for swellbility of the rubber in different solvents, the difference of polymer The degree of cross linking can quantitatively reflect that this illustrates that this method has higher practicality and higher accuracy by the above method.
Part is not directed to above, suitable for the prior art.
Although some specific embodiments of the present invention are described in detail by example, the skill of this area Art personnel it should be understood that above example merely to illustrate, the scope being not intended to be limiting of the invention, belonging to the present invention Those skilled in the art can make various modifications or additions or using class to described specific embodiment As mode substitute, but without departing from the direction or beyond the scope of the appended claims of the present invention.Ability Domain it is to be understood by the skilled artisans that it is every according to the present invention technical spirit embodiment of above is made any modification, etc. With replacement, improvement etc., protection scope of the present invention should be included in.

Claims (8)

  1. A kind of 1. test method of swell rubber degree, it is characterised in that:Comprise the following steps:
    (1), measure the quality of sample
    (2), will weigh after the sample be swollen under water-bath using solvent;
    (3), since the swelling every 20~24h measurements once sample quality, until adjacent measurement twice The difference of value is 0.01g~0.005g, and writing down the measured value is
  2. A kind of 2. test method of swell rubber degree as claimed in claim 1, it is characterised in that:The solvent is essential oil 2630th, Peppermint essential oil, one kind in coffee essential oil or at least two kinds.
  3. A kind of 3. test method of swell rubber degree as claimed in claim 1, it is characterised in that:The temperature range of the water-bath For 5~100 DEG C.
  4. A kind of 4. test method of swell rubber degree as claimed in claim 3, it is characterised in that:The temperature range of the water-bath For 20 DEG C~25 DEG C.
  5. A kind of 5. test method of swell rubber degree as claimed in claim 1, it is characterised in that:Surveyed using a ten thousandth balance Measure sample quality.
  6. A kind of 6. test method of swell rubber degree as claimed in claim 1, it is characterised in that:Step(3)In take out every time After sample, the solvent of sample surfaces attachment is blotted with filter paper rapidly, is immediately placed in measuring cup, weighs after covering tightly bottle stopper, then Put again in swelling pipe and continue to be swollen.
  7. A kind of 7. test method of swell rubber degree as claimed in claim 1, it is characterised in that:The quality of the sample Scope be 0.3~0.5g.
  8. A kind of 8. test method of swell rubber degree as claimed in claim 5, it is characterised in that:Step(1)It is additionally included in ten thousand First empty measuring cup is weighed on/mono- balance, then toward-block sample is put into measuring cup, is re-weighed, obtains the quality of sample
CN201711263286.2A 2017-12-05 2017-12-05 A kind of test method of swell rubber degree Pending CN108020481A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111562192A (en) * 2020-04-30 2020-08-21 江西安驰新能源科技有限公司 Evaluation method for swelling performance of binder for lithium battery
CN113008932A (en) * 2021-02-24 2021-06-22 常州汉韦聚合物有限公司 Method for correcting cross-linking degree test error
CN113092359A (en) * 2021-03-29 2021-07-09 湖北亿纬动力有限公司 Method for measuring swelling degree of glue for gluing diaphragm in electrolyte and application
CN113720723A (en) * 2021-08-26 2021-11-30 中国科学院广州地球化学研究所 Swelling method for kerogen

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103336109A (en) * 2013-05-31 2013-10-02 沈阳工业大学 Dynamic soaking swelling test device for rubber in liquid
CN105547896A (en) * 2015-12-11 2016-05-04 中北大学 Test method of crosslinking density of rubber foaming material
CN106226508A (en) * 2016-09-26 2016-12-14 国网四川省电力公司电力科学研究院 A kind of stretching device for swell rubber characteristic test and method of testing

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103336109A (en) * 2013-05-31 2013-10-02 沈阳工业大学 Dynamic soaking swelling test device for rubber in liquid
CN105547896A (en) * 2015-12-11 2016-05-04 中北大学 Test method of crosslinking density of rubber foaming material
CN106226508A (en) * 2016-09-26 2016-12-14 国网四川省电力公司电力科学研究院 A kind of stretching device for swell rubber characteristic test and method of testing

Non-Patent Citations (2)

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Title
中华人民共和国国家质量监督检验检疫总局 等: "《GB/T 1690-2006 硫化橡胶或热塑性橡胶耐液体试验方法》", 1 September 2006 *
王慧明 等: "原油温度对丁腈橡胶溶胀及耐磨损性能的影响", 《润滑与密封》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111562192A (en) * 2020-04-30 2020-08-21 江西安驰新能源科技有限公司 Evaluation method for swelling performance of binder for lithium battery
CN113008932A (en) * 2021-02-24 2021-06-22 常州汉韦聚合物有限公司 Method for correcting cross-linking degree test error
CN113092359A (en) * 2021-03-29 2021-07-09 湖北亿纬动力有限公司 Method for measuring swelling degree of glue for gluing diaphragm in electrolyte and application
CN113720723A (en) * 2021-08-26 2021-11-30 中国科学院广州地球化学研究所 Swelling method for kerogen

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Application publication date: 20180511

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