CN107189496A - A kind of modification illite preparation method for improving natural rubber performance - Google Patents
A kind of modification illite preparation method for improving natural rubber performance Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The present invention relates to a kind of modification illite preparation method for improving natural rubber performance, belong to Chemical Engineering and Technology field.The present invention is by illite powder and certain density mixed in hydrochloric acid and stirs, and using distilled water flushing and filters, the illite after acquisition pickling；Illite after pickling is blended with cetyl trimethylammonium bromide in 50% isopropanol water solution, and centrifugal drying obtains modified illite after reaction.The modification illite and natural rubber prepared using the present invention is mixed, and illite and native rubber composite material are obtained after vulcanization.The amount of loaded modified dose of modification illite prepared by the present invention is more, and compared with silane coupler prepares modified illite, its reaction time is shorter, and reaction temperature is relatively low.The cation modifier cetyl trimethylammonium bromide CTAB used in the present invention is more more cheap than silane coupler, the modification illite prepared with rubber disperse more preferably, mechanical property it is more outstanding.
Description
Technical field
The invention belongs to Chemical Engineering and Technology field, especially relate to a kind of modification for improving natural rubber performance she
Profit Preparation Method made of stones.
Background technology
Clay mixes rubber, can improve rubber mechanical property, reduces the cost of corresponding rubber product.Modified clay is in rubber
The ratio of middle addition is bigger, and the raising to rubber performance is also larger.The type clay be exactly use containing as amine, phosphorus, sulphur it is organic
Cation in thing, substitution clay particle layer, makes clay and rubber have more preferable affinity, especially dilatancy clay, it is easier to
It is modified and is adulterated with rubber, prepares corresponding composite.
Antu, Jilin Province finds a super-huge sandy non-expansibility Erie stone ore.City is applied to widen such a illite
, by the illite powder and blend rubber of certain mesh number, and physical performance is blended to it tested, result is that illite can be added
Amount is seldom.There is no much raisings to rubber performance.Reason be illite with blend rubber when it is scattered bad, easily reunite.Attempt
Property modified method, improve illitic performance, effect is not good, problem be in the layer of this illite particle spacing compared with
It is small, it is difficult to prize its interlayer spacing by traditional method of modifying.Organic matter group is brought in, improves existing illitic structure and property
Can, it is power of the invention to widen its application and usage amount.
Also there is other method to be modified for example silane coupler modified illite of illite at present, but due to illitic natural knot
Structure causes modified effect unobvious, and the content of modifying agent is relatively low.Illite is by two silicon-oxy tetrahedron sandwich, one aluminium
" TOT " structure that oxygen octahedra is constituted, wherein tetrahedron and octahedra connected by an oxygen atom are formed.Illitic
Different hydroxyls are dispersed with lamella, are largely that not reactive hydroxyl only has small part hydroxyl to participate in reaction.Eight
The oxygen atom not connected on the body piece of face with tetrahedron is combined aluminium hydroxyl, magnesium hydroxyl, iron that a hydrogen atom is formed in octahedron
Hydroxyl etc., these hydroxyls are can not to react hydroxyl.Reactive hydroxyl negligible amounts, only structure sheaf side in illite structure
Edge opens the silicone hydroxyl of formation of chemical bond, and a small amount of because the silicone hydroxyl that structure existing defects are produced is reactive hydroxyl.
Silane coupler modified illite needs largely participate in the hydroxyl of reaction, but because the hydroxyl quantity that illite can react
It is less, so the directly modified illite effect of silane coupler is weaker in method of modifying at present.Meanwhile, expensive silane coupler
Also a certain degree of influence is generated on the economic value of product.
Less using the directly modified illite method of cation modifier, modified effect is not obvious.Because illite
It is to belong to unexpansive clay cation modifier to strut illitic sandwich, can not while illite electronegativity is relatively low
Good Liquidity limit modifying agent, only a small amount of modifying agent is adsorbed at the tomography at illitic tomography edge.
Because modified illite has many difficulties, cause to improve also unobvious in the performance of composite, mechanical property
The properties increase rates such as energy are relatively low.
Therefore being needed badly among prior art wants a kind of new technical scheme to solve this problem.
The content of the invention
The technical problems to be solved by the invention are：A kind of modification illite preparation side for improving natural rubber performance is provided
Method make it that the content for being modified loaded modified dose of illite is more, improves the technical problem of illitic performance.One kind improves natural rubber
The modification illite preparation method of colloidality energy, comprises the following steps, and following steps are sequentially carried out,
Step 1: taking illite to deliver into mass concentration 0.5%~5%HCl solution, wherein solid-to-liquid ratio is 1 by g/ml：
40,1h~2h is stirred with 600rad/min in 50 DEG C~70 DEG C waters bath with thermostatic control, the illite after pickling is stood, normal temperature is down to
After filter；
Step 2: stirring is rushed repeatedly in three-necked flask by the illite deionized water after being filtered in the step one
Wash, until the deionized water pH value in three-necked flask is 7, be filtrated to get the illite after cleaning in blowing-type thermostatic drying chamber 60
Dried 24 hours under the conditions of DEG C, particle of claying into power, obtain illite powder after pickling；
Step 3: taking the pickling illite obtained in step 2 described in 5g, the isopropanol water solution of 200mL volumetric concentrations 50%
And 0.4g cetyl trimethylammonium bromides CTAB is added in 500ml there-necked flask reactors, in microwave and 70 DEG C~80 DEG C bars
0.5h~1h is reacted under part, stands to room temperature, uses centrifuge to centrifuge 5min under the conditions of 5000rad/min, consolidating after centrifugation
Determine particle and 24h is dried under the conditions of 60 DEG C of blowing-type thermostatic drying chamber, then illite is modified with the finely ground CTAB that obtains of agate mortar.
The particle diameter of powder particle in the step 2 is 0.5 μm~2 μm.
It is 0.5 μm~2 μm that the CTAB, which is modified illitic particle diameter,.
By above-mentioned design, the present invention can bring following beneficial effect：
Modified illitic new method is prepared the invention provides one kind, this method is obtained compared with original method of modifying
The content of modified loaded modified dose of illite increases.The modification illite prepared with this method of modifying made from rubber with being combined
Material and unmodified illite or original method be modified illite contrast this law preparation modification illite disperse in rubber compared with
The every excellent of composite that is good, obtaining, modification illite prepared by this law and conventional filler such as carbon black, silica pair
Than cheap.Modification illite prepared by this law is applied with very wide application prospect in rubber.
Modification illite prepared by the present invention is compared with silane coupler prepares modified illite, and its reaction time is shorter,
Reaction temperature is relatively low.The cation modifier cetyl trimethylammonium bromide CTAB used in the present invention is than silane coupler more
To be cheap.The modification illite that the present invention is prepared with rubber disperse more preferably, mechanical property it is more outstanding.
Brief description of the drawings
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated：
Fig. 1 is a kind of FB(flow block) for the modification illite preparation method for improving natural rubber performance of the present invention.
Fig. 2 is the illite after modified pickling in the present invention and is directly modified illitic thermal multigraph.
Fig. 3 is the illite after modified pickling in the present invention and is directly modified illitic infrared spectrogram.
Fig. 4 is raw ore illite surface scan electron microscope.
Fig. 5 is directly modified illite surface scan electron microscope.
Fig. 6 is illite surface scan electron microscope after pickling.
Fig. 7 is the illite surface scan electron microscope after modified pickling in the present invention.
Fig. 8 sweeps scanning electron microscope (SEM) photograph for the illite and native rubber composite material after the modified pickling of the present invention.
Fig. 9 is the illite and natural rubber composite wood X-ray diffraction light spectrogram after the modified pickling of the present invention.
The tensile property detection of illite and native rubber composite material that Figure 10 is prepared for embodiment three in the present invention is tied
Fruit is schemed.
A is directly modified illite thermogravimetric spectral line in figure, and b is the illite thermogravimetric spectral line after modified pickling, c for raw ore she
Sharp stone infrared spectrogram, d is directly modified illite infrared spectrogram, and e is the illite infrared spectrogram after modified pickling, f
For natural rubber X-ray diffraction light spectrogram, g is directly modified illite and natural rubber X-ray diffraction light spectrogram, h for after pickling she
Sharp stone and natural rubber X-ray diffraction light spectrogram.
Embodiment
Embodiment one,
A kind of modification illite preparation method for improving natural rubber performance, comprises the following steps, and following steps are suitable
It is secondary to carry out,
Step 1: taking illite to deliver into mass concentration 0.5%HCl solution, wherein solid-to-liquid ratio is 1 by g/ml：40,
1.5h is stirred with 600rad/min in 50 DEG C of waters bath with thermostatic control, the illite after pickling is stood, is down to after normal temperature and filters；
Step 2: stirring is rushed repeatedly in three-necked flask by the illite deionized water after being filtered in the step one
Wash, until the deionized water pH value in three-necked flask is 7, be filtrated to get the illite after cleaning in blowing-type thermostatic drying chamber 60
Dried 24 hours under the conditions of DEG C, particle of claying into power, obtain illite powder after pickling；
Step 3: taking the pickling illite obtained in step 2 described in 5g, the isopropanol water solution of 200mL volumetric concentrations 50%
It is anti-under the conditions of microwave and 70 DEG C and 0.4g cetyl trimethylammonium bromides CTAB is added in 500ml there-necked flask reactors
0.5h is answered, stands to room temperature, uses centrifuge to centrifuge 5min under the conditions of 5000rad/min, the fixation particle after centrifugation is in drum
24h is dried under the conditions of 60 DEG C of wind formula thermostatic drying chamber, then illite is modified with the finely ground CTAB that obtains of agate mortar.
The particle diameter of powder particle in the step 2 is 0.5 μm~2 μm.
It is 0.5 μm~2 μm that the CTAB, which is modified illitic particle diameter,.
Embodiment two,
A kind of modification illite preparation method for improving natural rubber performance, comprises the following steps, and following steps are suitable
It is secondary to carry out,
Step 1: taking illite to deliver into mass concentration 5%HCl solution, wherein solid-to-liquid ratio is 1 by g/ml：40,70
2h is stirred with 600rad/min in DEG C water bath with thermostatic control, the illite after pickling is stood, is down to after normal temperature and filters；
Step 2: stirring is rushed repeatedly in three-necked flask by the illite deionized water after being filtered in the step one
Wash, until the deionized water pH value in three-necked flask is 7, be filtrated to get the illite after cleaning in blowing-type thermostatic drying chamber 60
Dried 24 hours under the conditions of DEG C, particle of claying into power, obtain illite powder after pickling；
Step 3: taking the pickling illite obtained in step 2 described in 5g, the isopropanol water solution of 200mL volumetric concentrations 50%
It is anti-under the conditions of microwave and 75 DEG C and 0.4g cetyl trimethylammonium bromides CTAB is added in 500ml there-necked flask reactors
0.8h is answered, stands to room temperature, uses centrifuge to centrifuge 5min under the conditions of 5000rad/min, the fixation particle after centrifugation is in drum
24h is dried under the conditions of 60 DEG C of wind formula thermostatic drying chamber, then illite is modified with the finely ground CTAB that obtains of agate mortar.
The particle diameter of powder particle in the step 2 is 0.5 μm~2 μm.
It is 0.5 μm~2 μm that the CTAB, which is modified illitic particle diameter,.
Embodiment three：
First, modified illite is prepared：
10g illites are taken to deliver into 1%HCl solution, solid-to-liquid ratio is 1 by g/ml：40,60 DEG C of waters bath with thermostatic control, 600rad/
Min stirs 1h, is filtered after the illite standing, cooling after pickling；
With deionized water, stirring rinses multiple repeatedly in three-necked flask, until pH value is 7, is filtrated to get sample drying 24
After hour, particle of claying into power obtains illite after pickling；
The above-mentioned pickling illites of 5g are taken, 200mL volumetric concentrations are that 50% isopropanol water solution and 0.4gCTAB are added
In 500ml there-necked flask reactors.Centrifugation under the conditions of 1h, standing to room temperature, 5000rad/min is reacted under the conditions of microwave and 80 DEG C
5min, 60 DEG C of dry 24h, then it is modified illite with the finely ground CTAB that obtains of agate mortar.
2nd, illite and native rubber composite material are prepared
Refine quality of material ratio：Rubber 100, sulphur 2.5, accelerator (diphenylguanidine) 1, zinc oxide 5, stearic acid 1, modified Erie
Stone flour 0~20.
Elastomeric compound prepares as shown in table 1：Torque rheometer capacity 200ml, 70 DEG C of banbury initial temperature, rotor speed
60rad/min。
It can be seen that method disclosed by the invention increases the content of loaded modified dose of illite from Fig. 2 and Fig. 3.From figure
Cetyl trimethylammonium bromide CTAB is can see in 4 to Fig. 7 contrasts with graininess on illite surface.Table 2 is the present invention
Illite and directly modified illitic mechanical property correction data table after modified pickling.It can be seen that this method from table 2
Modified illite and rubber composite properties are modified illite better than conventional method.The modified illite of the present invention exists
It is well mixed in rubber and does not form reunion as shown in Figure 8.The modified illite of present invention dispersive property in rubber is better than Erie
Stone disperses as shown in Figure 9 in rubber.The illite prepared to embodiment three is detected with native rubber composite material tensile property
As a result it is as shown in Figure 10.
The operating process of table 1
Table 2 is modified the illite after pickling and is directly modified illitic mechanical property correction data table
Applicant states that the present invention illustrates the method detailed of the present invention by examples detailed above, but the present invention is not limited to
Above-mentioned method detailed, that is, do not mean that the present invention has to rely on above-mentioned method detailed and could implemented.The technology of art
Personnel are it will be clearly understood that any to the present invention improve, to product of the present invention and the change of Feedstock treating condition and the replacement of raw material and auxiliary
The addition of co-ingredients, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and being open.
Claims (3)
1. a kind of modification illite preparation method for improving natural rubber performance, it is characterized in that：Comprise the following steps, and below
Step is sequentially carried out,
Step 1: taking illite to deliver into mass concentration 0.5%~5%HCl solution, wherein solid-to-liquid ratio is 1 by g/ml：40,
1h~2h is stirred with 600rad/min in 50 DEG C~70 DEG C waters bath with thermostatic control, the illite after pickling is stood, is down to after normal temperature
Filtering；
Step 2: by the illite deionized water after being filtered in the step one, stirring is rinsed repeatedly in three-necked flask, directly
Deionized water pH value into three-necked flask is 7, is filtrated to get the illite after cleaning in 60 DEG C of bars of blowing-type thermostatic drying chamber
Dried 24 hours under part, particle of claying into power, obtain illite powder after pickling；
Step 3: take the pickling illite obtained in step 2 described in 5g, the isopropanol water solution of 200mL volumetric concentrations 50% and
0.4g cetyl trimethylammonium bromides CTAB is added in 500ml there-necked flask reactors, under the conditions of microwave and 70 DEG C~80 DEG C
0.5h~1h is reacted, stands to room temperature, uses centrifuge to centrifuge 5min under the conditions of 5000rad/min, the fixation after centrifugation
Grain dries 24h under the conditions of 60 DEG C of blowing-type thermostatic drying chamber, then is modified illite with the finely ground CTAB that obtains of agate mortar.
2. a kind of modification illite preparation method for improving natural rubber performance according to claim 1, it is characterized in that：Institute
The particle diameter for stating the powder particle in step 2 is 0.5 μm~2 μm.
3. a kind of modification illite preparation method for improving natural rubber performance according to claim 1, it is characterized in that：Institute
It is 0.5 μm~2 μm to state CTAB in step 3 and be modified illitic granularity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694486A (en) * | 2018-11-20 | 2019-04-30 | 北京化工大学 | The preparation method of 100% γ phase PVDF thin film |
| CN115948058A (en) * | 2023-02-21 | 2023-04-11 | 浙江职信通信科技有限公司 | Preparation method of antibacterial and deodorant plastic modified material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109694486A (en) * | 2018-11-20 | 2019-04-30 | 北京化工大学 | The preparation method of 100% γ phase PVDF thin film |
| CN109694486B (en) * | 2018-11-20 | 2022-10-14 | 北京化工大学 | Preparation method of 100% gamma-phase PVDF film |
| CN115948058A (en) * | 2023-02-21 | 2023-04-11 | 浙江职信通信科技有限公司 | Preparation method of antibacterial and deodorant plastic modified material |
| CN115948058B (en) * | 2023-02-21 | 2024-02-27 | 浙江职信通信科技有限公司 | Preparation method of antibacterial and deodorant plastic modified material |
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