CN109596451A - The detection method of insoluble matter in bibasic ethylene propylene rubber - Google Patents
The detection method of insoluble matter in bibasic ethylene propylene rubber Download PDFInfo
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- CN109596451A CN109596451A CN201710915721.9A CN201710915721A CN109596451A CN 109596451 A CN109596451 A CN 109596451A CN 201710915721 A CN201710915721 A CN 201710915721A CN 109596451 A CN109596451 A CN 109596451A
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- G—PHYSICS
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of detection methods of insoluble matter in bibasic ethylene propylene rubber.Detection method includes the following steps: S1 for this, weighs bibasic ethylene propylene rubber and is dissolved in base oil 150N；S2 is filtered with the strainer that filtering accuracy is 1~75 μm, strainer is then amplified observation by the method for electron microscope and photograph, is checked whether with the presence of insoluble matter, if any presence, then utilizes the content for the method test insoluble matter for weighing loss of weight.It applies the technical scheme of the present invention, it is filtered first with strainer, then strainer is amplified into observation by the method for electron microscope and photograph, thus more can quickly it judge in bibasic ethylene propylene rubber with the presence or absence of Superhigh Molecular Polymer, if it is observed that insoluble matter has presence under microscope, then using the content for the method test insoluble matter for weighing loss of weight, insolubles content is calculated so as to more accurate.
Description
Technical field
The present invention relates to EP rubbers technical fields, in particular to a kind of inspection of insoluble matter in bibasic ethylene propylene rubber
Survey method.
Background technique
The production technology of domestic and international EP rubbers mainly has polymerisation in solution, suspension polymerisation and gas-phase polymerization etc., wherein solution
Polymerization technique accounts for the 80% of world's total output energy.In recent years, the development of polymerization technique is mainly reflected in the update of catalyst,
By vanadium-aluminium of traditional ziegler-nata vanadium catalysis system, titanium-aluminium homogeneous catalyst to vanadium, titanium carrier catalyst, so far with
Metallocene, non-cyclopentadienyl single center catalyst system production technology be also gradually improved；And traditional ziegler-nata vanadium-aluminium is homogeneously urged
Change system, although catalytic efficiency (102-103Kg glue/g catalyst) it is lower, but the technical indicators such as ENB, Mooney viscosity can be produced
The EP rubbers of all trades mark from low to high, and technology maturation, production is stablized, currently, the 76% of EP rubbers world production capacity
It is all using this catalyst system above.
Lubricating oil viscosity index improver is one of bibasic ethylene propylene rubber main application, domestic internal combustion engine lubrication in 2012
It is 4,000,000 tons that oil meter, which sees consumption, needs 20,000 tons of EP rubbers according to the calculating of 0.5% adding rate.Domestic Jilin Petrochemical is being introduced
Mitsui company produces self-developing development on the basis of 20,000 tons of EP rubbers per year, mainly there is J-0080, J-0050, J- at present
0030, tetra- trades mark of J-0010.Its molecular weight of J-0010 is low, and relative molecular mass distribution is narrow, and shear stability is good, and the product is not
It needs to degrade, is directly used in modulation top-grade lubricating oil.
In process of production, polymerization technique control is stringenter for traditional ziegler-nata vanadium-aluminium homogeneous catalysis system,
Otherwise a large amount of gel can be generated or have insoluble matter insoluble in lubricating oil to occur, but from the appearance of product and routine test index
In be difficult find and detect, conventional gel test method can not embody completely the content of insoluble matter in second third, and distinguish
It is tested in the analysis of lubricating oil oil product insoluble matter.
Analysis test to bibasic ethylene propylene rubber insoluble matter, substantially with the test method of high molecular polymer gel content
It carries out, this method cannot rapidly and accurately reflect whether the third polymer of second contains insoluble matter, can not accurately test it
The content of insoluble matter.
Summary of the invention
The present invention is intended to provide in a kind of bibasic ethylene propylene rubber insoluble matter detection method, with solve in the prior art to two
The technical issues of first EP rubbers cannot quickly judge whether containing insoluble matter.
To achieve the goals above, according to an aspect of the invention, there is provided insoluble matter in a kind of bibasic ethylene propylene rubber
Detection method.Detection method includes the following steps: S1 for this, weighs bibasic ethylene propylene rubber and is dissolved in base oil 150N；S2 is used
Filtering accuracy is that 1~75 μm of strainer is filtered, and then amplifies strainer by electron microscope and the method for photograph
Observation is checked whether with the presence of insoluble matter, if any presence, then utilizes the content for the method test insoluble matter for weighing loss of weight.
Further, in step S1, the mass ratio of bibasic ethylene propylene rubber and base oil 150N are 1~15%.
Further, under 80~140 DEG C, the rotation condition that agitation revolution is 130~170 revs/min, by binary second third
Rubber solution is in base oil 150N, until being completely dissolved.
Further, the object of insoluble analyte detection includes gel and weight average molecular weight is more than 106Superhigh Molecular Polymer.
Further, Superhigh Molecular Polymer is observed and is clapped under conditions of electron microscope amplifies 400 times
According to.
Further, it is required according to OIL IN LUBRICATING OIL PRODUCTION technique, changes the aperture of filter screen.
Further, S2 is specifically included: S21, has weighed strainer two, is filtered and is dissolved with a piece of strainer therein
Bibasic ethylene propylene rubber liquid, after 100g glue all filtering, glue on empty clean strainer is uniform by the retentate on strainer
The painting on piece for being coated onto electron microscope, be amplified to 400 times and observed and taken pictures；S22 repeats remaining another strainer
The strainer of empty clean oil product is placed in Soxhlet extractor by filter, and toluene is added, control toluene under the conditions of boiling into
Row reflux dissolution took out strainer after 2~8 hours, weighing strainer weight was carried out after toluene volatilize completely, using clean
Strainer and reflux after strainer weight difference, calculate the insolubles content of the third glue of binary second.
Further, bibasic ethylene propylene rubber is using vanadium-aluminium catalyst system as catalyst system, and polymerization technique is polymerisation in solution
The bibasic ethylene propylene rubber being polymerized.
Further, polymerized monomer is ethylene and propylene in polymerization technique.
It applies the technical scheme of the present invention, is filtered first with strainer, strainer is then passed through into electron microscope and photograph
The method of phase amplifies observation, thus more can quickly judge in bibasic ethylene propylene rubber with the presence or absence of supra polymer
Polymer then utilizes the content for the method test insoluble matter for weighing loss of weight if it is observed that insoluble matter has presence under microscope.Separately
Outside, solidifying if there is high molecular polymer can be used for reference because being can decide whether from microscope there are Superhigh Molecular Polymer
Glue content assaying method determines the test method of insoluble matter in the third polymer of second, finds suitable solvent, suitable the third glue of second
Concentration and return time are different from the gel test method of original high polymer, so as to it is more accurate calculate it is insoluble
Object content.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the Microscopy Results of embodiment 1；
Fig. 2 shows the Microscopy Results of embodiment 2；
Fig. 3 shows the Microscopy Results of embodiment 3；And
Fig. 4 shows the Microscopy Results of embodiment 4；.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
A kind of typical embodiment according to the present invention provides a kind of detection method of insoluble matter in bibasic ethylene propylene rubber.
Detection method includes the following steps: S1 for this, weighs bibasic ethylene propylene rubber and is dissolved in base oil 150N；S2 is 1 with filtering accuracy
~75 μm of strainer is filtered, and strainer is then amplified observation by the method for electron microscope and photograph, checking is
It is no with the presence of insoluble matter, if any presence, then utilize the content for the method test insoluble matter for weighing loss of weight.
It applies the technical scheme of the present invention, is filtered first with strainer, strainer is then passed through into electron microscope and photograph
The method of phase amplifies observation, thus can accurately judge in bibasic ethylene propylene rubber with the presence or absence of supra polymer
Polymer observes that insoluble substance has presence as crossed under microscope, then using the content for the method test insoluble matter for weighing loss of weight, from
And can be more accurate calculate insolubles content.
Preferably, in step S1, the mass ratio of bibasic ethylene propylene rubber and base oil 150N are 1~15%.Within this range,
Bibasic ethylene propylene rubber can be made sufficiently to dissolve, and be unlikely to make insoluble matter excess dilution.
Preferably, under conditions of agitation revolution is 130~170 revs/min, bibasic ethylene propylene rubber is molten at 80~140 DEG C
Solution is in base oil 150N, until being completely dissolved.Efficiently bibasic ethylene propylene rubber can be dissolved under the conditions of this temperature and revolution
In base oil 150N.
A kind of typical embodiment, the object of insoluble analyte detection include gel and Superhigh Molecular Polymer according to the present invention
(weight average molecular weight is more than 106)。
Preferably, Superhigh Molecular Polymer is observed and is taken pictures under conditions of electron microscope amplifies 400 times.?
It is easy whether to recognize with the presence of insoluble matter under this condition.
A kind of typical embodiment according to the present invention requires according to OIL IN LUBRICATING OIL PRODUCTION technique, changes the aperture of filter screen,
Quickly detect the content of insoluble matter.
Preferably, S2 is specifically included: S21, has weighed strainer 2, is filtered with a piece of strainer therein and have been dissolved
Bibasic ethylene propylene rubber liquid, after 100g glue all filtering, glue on empty clean strainer is uniform by the retentate on strainer
It is coated onto the painting on piece of electron microscope, 400 times is amplified to and is observed and taken pictures；S22 repeated remaining another strainer
The strainer of empty clean oil product is placed in Soxhlet extractor by filter fly sequence, and toluene is added, and control toluene carries out under the conditions of boiling
Reflux dissolution took out strainer after 2~8 hours, weighing strainer weight was carried out after toluene volatilize completely, using clean
The weight difference of strainer after strainer and reflux, calculates the insolubles content of the third glue of binary second.
A kind of typical embodiment according to the present invention, bibasic ethylene propylene rubber are using vanadium-aluminium catalyst system as catalytic body
System, polymerization technique are the bibasic ethylene propylene rubber that polymerisation in solution is polymerized, and polymerized monomer is ethylene and propylene.
A kind of typical embodiment according to the present invention, the detection method of insoluble matter is specific as follows in bibasic ethylene propylene rubber:
1) qualitative analysis is carried out to strainer using micro- sem observation and the method for photograph；
First by load weighted bibasic ethylene propylene rubber, be put into the 150N base oil of certain temperature, under agitation into
The dissolution of row constant temperature stops heating and stirring after range estimation blob of viscose is dissolved completely in base oil, and the glue dissolved is naturally cold
But room temperature is arrived, can be filtered with the strainer of different meshes, the naturally empty net glue of the strainer after then using filtering will be on strainer
Insoluble matter to be measured carries out smear processing, with electron microscope observation, in the presence of having insoluble matter, it is seen that clearly size is not
Same, irregular pattern different in size is distributed in painting on piece, and shade is different, in the presence of no insoluble matter, it is seen that uniform
Picture and color is uniform；
2) carrying out quantitative analysis to the insoluble matter on strainer can be used the method for weighing loss of weight；
The strainer of empty clean oil product is placed in Soxhlet extractor, a certain amount of toluene is added, control toluene is boiling
Under the conditions of carry out reflux dissolution, by after a certain period of time, take out strainer, weighing strainer weight carried out after toluene volatilize completely,
Using the weight difference of the strainer after clean strainer and reflux, the insolubles content of a certain amount of the third glue of second is calculated.
Technical solution of the present invention is suitable for the bibasic ethylene propylene rubber using solution polymerization process preparation；Suitable for polymerizeing work
Skill is with n-hexane, hexamethylene, benzene and other C5~C8Hydrocarbon etc. is the ethylene propylene polymerization object of solvent；Suitable for polymerization technique with neat
The Natta-catalyzed system of Ge Le-is the ethylene propylene polymerization object of catalyst；It is adapted to conform with all trade mark ethylene propylenes of above-mentioned condition
Alkene polymer；The ethylene propylene polymerization object of this method analysis is the final products of EP rubbers production process.
The analysis result of this method can production to EP rubbers, technology controlling and process play the role of auxiliary and guidance, and it is right
Lubrication oil Production Process provides directive function.In addition, insoluble object detecting method, analog production procedure, predict lubricating oil in life
The stifled extension situation of filter bag during production.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
The 150N base oil of 180g is added in the there-necked flask of 500ml, is warming up to 80 DEG C, agitation revolution 120rpm, accurately
20g bibasic ethylene propylene rubber is weighed, is put into there-necked flask after chopping, is gradually warmed up to 120~140 DEG C, constant temperature stirring 3~10 is small
When, exist when observing without obvious insoluble matter, when glue is transparent and homogeneous shape, stops heating and stirring, naturally cool to room temperature.
With strainer 2 of the 75um for weighing good certain area, it is filtered and is dissolved with a piece of clean strainer therein
The third glue of second, after 100g glue all filtering, the retentate on strainer is uniformly coated by glue on empty clean strainer
The painting on piece of electron microscope is amplified to 400 times and is observed and taken pictures, as a result as shown in Figure 1.
Remaining another clean strainer is repeated into above-mentioned filter, the glue on empty clean strainer, after filtering
Strainer be placed in Soxhlet extractor, be added 50 ± 0.2ml toluene, control toluene carry out flowing back under the conditions of boiling it is molten
Solution takes out strainer by after a certain period of time, carries out weighing strainer weight after toluene volatilize completely, using clean strainer and
The weight difference of strainer after reflux calculates the insolubles content of a certain amount of the third glue of second.
Insolubles content is indicated with its mass percent, is calculated by following formula, and one decimal place is as a result accurate to:
In formula: W- insolubles content is calculated in mass percent, %；
m0Sample mass, g；
mlFilter quality, g；
m2Filter adds insoluble matter quality, g.
Tolerance:
When insolubles content is less than 1.0%, the difference of parallel determinations is not more than 0.2% twice；
For insolubles content at 1.1%~2.0%, the difference of parallel determinations is not more than 0.5% twice.
W=0.58% in the present embodiment.
Embodiment 2
The 150N base oil of 180g is added in the there-necked flask of 500ml, is warming up to 80 DEG C, agitation revolution 120rpm, accurately
20g bibasic ethylene propylene rubber is weighed, is put into there-necked flask after chopping, is gradually warmed up to 120~140 DEG C, constant temperature stirring 3~10 is small
When, exist when observing without obvious insoluble matter, when glue is transparent and homogeneous shape, heating and stirring can be stopped, naturally cooling to room
Temperature.
With strainer 2 of the 25um for weighing good certain area, it is filtered and is dissolved with a piece of clean strainer therein
The third glue of second, after 100g glue all filtering, the retentate on strainer is uniformly coated by glue on empty clean strainer
The painting on piece of electron microscope is amplified to 400 times and is observed and taken pictures, as a result as shown in Fig. 2, calculating W=2.4%.
Embodiment 3
The 150N base oil of 180g is added in the there-necked flask of 500ml, is warming up to 80 DEG C, agitation revolution 120rpm, accurately
20g bibasic ethylene propylene rubber is weighed, is put into there-necked flask after chopping, is gradually warmed up to 120~140 DEG C, constant temperature stirring 3~10 is small
When, exist when observing without obvious insoluble matter, when glue is transparent and homogeneous shape, heating and stirring can be stopped, naturally cooling to room
Temperature.
With strainer 2 of the 10um for weighing good certain area, it is filtered and is dissolved with a piece of clean strainer therein
The third glue of second, after 100g glue all filtering, the retentate on strainer is uniformly coated by glue on empty clean strainer
The painting on piece of electron microscope is amplified to 400 times and is observed and taken pictures, as a result as shown in figure 3, calculating W=5.4%
Embodiment 4
The 150N base oil of 180g is added in the there-necked flask of 500ml, is warming up to 80 DEG C, agitation revolution 120rpm, accurately
20g bibasic ethylene propylene rubber is weighed, is put into there-necked flask after chopping, is gradually warmed up to 120~140 DEG C, constant temperature stirring 3~10 is small
When, exist when observing without obvious insoluble matter, when glue is transparent and homogeneous shape, heating and stirring can be stopped, naturally cooling to room
Temperature.
With strainer 2 of the 10um for weighing good certain area, it is filtered and is dissolved with a piece of clean strainer therein
The third glue of second, after 100g glue all filtering, the retentate on strainer is uniformly coated by glue on empty clean strainer
The painting on piece of electron microscope is amplified to 400 times and is observed and taken pictures, as a result as shown in figure 4, calculating W=0.3%
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: first with rule
Fixed strainer is filtered, and strainer is then amplified observation by the method for electron microscope and photograph, thus can be with
More quickly judge to whether there is Superhigh Molecular Polymer in bibasic ethylene propylene rubber, observes insoluble matter as crossed under microscope
There is presence, then using the test method of patent test insoluble matter, using defined solvent and dissolving method, with the side for weighing loss of weight
Method tests the content of insoluble matter, calculates insolubles content so as to more accurate.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. the detection method of insoluble matter in a kind of bibasic ethylene propylene rubber, which comprises the following steps:
S1 weighs bibasic ethylene propylene rubber and is dissolved in base oil 150N；
S2 is that 1~75 μm of strainer is filtered with filtering accuracy, and the strainer is then passed through electron microscope and photograph
Method amplifies observation, checks whether with the presence of insoluble matter, if any presence, then tests insoluble matter using the method for weighing loss of weight
Content.
2. detection method according to claim 1, which is characterized in that in the step S1, bibasic ethylene propylene rubber and basis
The mass ratio of oily 150N is 1~15%.
3. detection method according to claim 1, which is characterized in that at 80~140 DEG C, agitation revolution is 130~170
Rev/min rotation condition under, bibasic ethylene propylene rubber is dissolved in base oil 150N, until being completely dissolved.
4. detection method according to claim 1 again, which is characterized in that the object of insoluble analyte detection includes gel and divides equally
Son amount is more than 106Superhigh Molecular Polymer.
5. detection method according to claim 4, which is characterized in that the Superhigh Molecular Polymer in electron microscope
Under conditions of 400 times of amplification, is observed and taken pictures.
6. detection method according to claim 4, which is characterized in that required according to OIL IN LUBRICATING OIL PRODUCTION technique, change filtering
The aperture of net.
7. detection method according to claim 1, which is characterized in that the S2 is specifically included:
S21 has weighed strainer two, the bibasic ethylene propylene rubber liquid dissolved is filtered with a piece of strainer therein, by 100g
Glue is all after filtering, and the retentate on strainer is uniformly coated onto the smear of electron microscope by the glue on empty clean strainer
On, it is amplified to 400 times and is observed and taken pictures；
Remaining another strainer is repeated filter by S22, and the strainer of empty clean oil product is placed in Soxhlet extractor,
Toluene is added, control toluene carries out reflux dissolution under the conditions of boiling, after 2~8 hours, takes out strainer, complete to toluene
Weighing strainer weight is carried out after volatilization calculates the third glue of binary second using the weight difference of the strainer after clean strainer and reflux
Insolubles content.
8. detection method according to claim 1, which is characterized in that the bibasic ethylene propylene rubber is with vanadium-aluminium catalytic body
System is used as catalyst system, and polymerization technique is the bibasic ethylene propylene rubber that polymerisation in solution is polymerized.
9. detection method according to claim 8, which is characterized in that polymerized monomer is ethylene and third in the polymerization technique
Alkene.
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Cited By (1)
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| CN114428077A (en) * | 2020-09-30 | 2022-05-03 | 中国石油化工股份有限公司 | Method for analyzing rubber particles in polymer material |
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