CN108129693A - Oil-filled type insoluble sulfur and its preparation method and application - Google Patents
Oil-filled type insoluble sulfur and its preparation method and application Download PDFInfo
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- CN108129693A CN108129693A CN201711415263.9A CN201711415263A CN108129693A CN 108129693 A CN108129693 A CN 108129693A CN 201711415263 A CN201711415263 A CN 201711415263A CN 108129693 A CN108129693 A CN 108129693A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The present invention provides a kind of oil-filled type insoluble sulfurs and its preparation method and application, are related to the technical field of vulcanizing agent preparation.The preparation method of the oil-filled type insoluble sulfur, by the way that stabilizer and filling oil are mixed to get paste, then paste and insoluble sulfur are mixed to get oil-filled type insoluble sulfur, with good thermal stability and dispersibility, optimize product performance, the technical issues of oil-filled type insoluble sulfur quality for solving the preparation method of oil-filled type insoluble sulfur in the prior art and being prepared is bad reaches the standard of the external same industry, is expected to break the monopolization of foreign country.
Description
Technical field
The present invention relates to vulcanizing agent preparing technical field, more particularly, to a kind of oil-filled type insoluble sulfur and its preparation side
Method and application.
Background technology
Sulphur is the important vulcanizing agent of rubber, and the common sulphur of rubber compounding is stable rhomboidal crystal, processing and
Rubber hydrocarbon is dissolved under curing temperature, but as sizing material cools down in parking period, sulphur rapidly diffuses into sizing material surface simultaneously
Crystallization, causes surface sulfuring up.This sulfuring up can influence bonding between the processing performance of sizing material and performance, such as cord etc..
Insoluble sulfur (Insoluble Sulfur), abbreviation IS, be sulphur chain polymer, because insoluble in carbon disulfide
It gains the name with rubber hydrocarbon.Insoluble sulfur is widely used in mainly as the advanced accelerating agent and vulcanizing agent of a kind of rubber industry
In the manufacturing of tire and other rubber composite products, the carcass sizing material of such as tire buffers sizing material, white sidewall rubber and turns over
In the sizing material that the rubber such as tire, sebific duct, adhesive tape are bonded with framework material, it can also be used to the rubber systems such as cable, rubber roller, oil sealing, rubber overshoes
In the sizing material of product, while it is also applied in the big light-colour rubber product of sulfur consumption.Since insoluble sulfur can make meridian, steel
Silk and rubber stickup are more secured, effectively prevent sizing material crocking, improve heat-resisting, the wear-resisting property of tire.Therefore, insoluble sulfur is
Essential important source material in tire production.Insoluble sulfur is because of the characteristic of its linear polymeric, insoluble in rubber, Bu Huiqian
Sizing material surface is moved on to, sulfuring up will not be generated, insoluble sulfur can also improve the white viscosity of sizing material, improve rubber layer and layer
Between adhesive strength, insoluble sulfur can shorten curing cycle, and tire wear resistance is good made of insoluble sulfur, compared to general
Logical tire improves 30%-50%, and 1.5 times that service life is conventional tyre.
Insoluble sulfur product will generally carry out Oil treatment.But use, which is not achieved, in domestic quality index for a long time wants
It asks, particularly 120 DEG C of stability, the domestic market of oil-filled type insoluble sulfur is monopolized by foreign country, to the hair of domestic tyre industry
Exhibition brings bottleneck, and with the improvement of road traffic and the development of automobile technology, the rapid growth of radial drives significantly
The demand of insoluble sulfur.Product severe relies on import.Therefore, a kind of oil-filled type prepared with good thermal stability is insoluble
The preparation method of sulphur and a kind of oil-filled type insoluble sulfur with good thermal stability are that existing market is highly desirable.
In view of this, it is special to propose the present invention.
Invention content
The first object of the present invention is to provide a kind of preparation method of oil-filled type insoluble sulfur solve the prior art
Present in oil-filled type insoluble sulfur preparation method prepare the technology of oil-filled type insoluble sulfur thermal stability difference arrived
Problem.
The second object of the present invention is to provide a kind of oil-filled type insoluble sulfur, solve it is in the prior art by
The technical issues of oil-filled type insoluble sulfur thermal stability that prior art preparation obtains is poor.
The third object of the present invention is to provide a kind of application of above-mentioned oil-filled type insoluble sulfur in the vulcanization of rubber, solve
A kind of oil-filled type insoluble sulfur that can prepare good thermal stability of shortage in the prior art determined in the vulcanization of rubber
In application the technical issues of.
The fourth object of the present invention is to provide a kind of method of the vulcanization of rubber, and this method is insoluble using above-mentioned oil-filled type
Sulphur, the oil-filled type that a kind of good thermal stability is lacked in the method for solving the vulcanization of rubber in the prior art are insoluble
The technical issues of sulphur.
In order to solve the above technical problems, spy of the present invention adopts the following technical scheme that：
A kind of preparation method of oil-filled type insoluble sulfur, the preparation method include the following steps：By stabilizer with filling out
It is oil-filled to be mixed to get paste, then gained paste with insoluble sulfur is mixed, oil-filled type insoluble sulfur is prepared；
Wherein, the stabilizer includes dibenzothiazyl disulfide, PR-75 type rubber disperse agent and PR-85 types rubber point
It is one or more in powder；
Preferably, the stabilizer is dibenzothiazyl disulfide and the stable composition of PR-75 type rubber disperses agent composition
The compound stabilizer of agent or dibenzothiazyl disulfide and PR-85 type rubber disperses agent composition.
Further, the dosage of the dibenzothiazyl disulfide is the 0.2%-0.9% of insoluble sulfur quality, described
The dosage of PR-75 type rubber disperse agent is the 0.3%-0.8% of insoluble sulfur quality, the PR-85 types rubber disperse agent
Dosage is the 0.3%-0.8% of insoluble sulfur quality；
Preferably, the dosage of the dibenzothiazyl disulfide is the 0.3%-0.6% of insoluble sulfur quality, described
The dosage of PR-75 type rubber disperse agent is the 0.5%-0.7% of insoluble sulfur quality, the PR-85 types rubber disperse agent
Dosage is the 0.5%-0.7% of insoluble sulfur quality；
It is further preferred that the dosage of the dibenzothiazyl disulfide is the 0.4% of insoluble sulfur quality, it is described
The dosage of PR-75 type rubber disperse agent is the 0.6% of insoluble sulfur quality, and the dosage of the PR-85 types rubber disperse agent is
The 0.55% of insoluble sulfur quality.
Further, the mass fraction of insoluble sulfur is 90%-100% in the insoluble sulfur.
Further, the dosage of the filling oil is the 2%-33% of insoluble sulfur quality；
Preferably, the dosage of the filling oil is the 10%-30% of insoluble sulfur quality；
It is further preferred that the dosage of the filling oil is the 20% of insoluble sulfur quality.
Further, the preparation method may further include the step of crushing insoluble sulfur before mixing；
Preferably, it is that insoluble sulfur is crushed to 50-150 mesh.
Further, the paste and the insoluble sulfur incorporation time are 10-30min.
A kind of oil-filled type insoluble sulfur, the oil-filled type insoluble sulfur are prepared by above-mentioned preparation method.
Further, 120 DEG C of thermal stability of the oil-filled type insoluble sulfur is 45%-60%.
A kind of application of above-mentioned oil-filled type insoluble sulfur in the vulcanization of rubber.
A kind of method of the vulcanization of rubber uses above-mentioned oil-filled type insoluble sulfur in this method.
Beneficial effects of the present invention are：The preparation method of oil-filled type insoluble sulfur provided by the invention, by that will stablize
Agent is mixed to get paste with filling oil, and paste and insoluble sulfur then are mixed to get oil-filled type insoluble sulfur, this
Stabilizer in the technical solution provided is provided and uses dibenzothiazyl disulfide, PR-75 type rubber disperse agent and PR-85 type rubber
One or more in dispersant, it is preferable to use dibenzothiazyl disulfide and PR-75 type rubber disperses agent composition it is compound steady
Determine the compound stabilizer of agent or dibenzothiazyl disulfide and PR-85 type rubber disperses agent composition.Oil-filled type made from this method
Insoluble sulfur has good thermal stability, can will be 120 DEG C former, 15min stability is 30%, improves more than 45%, from
And the existing requirement of high stability insoluble sulfur for meeting all-steel radial tyre production requirement is met and exceeded, and into one
Step integrates the granularity of insoluble sulfur, and the particle size distribution of insoluble sulfur is made further to concentrate, improves dispersibility, optimizes
Product performance.Oil-filled type insoluble sulfur provided by the invention is prepared using the above method, has good 120
DEG C, 15min thermal stability reaches the standard of the external same industry, has broken the monopolization of foreign country.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution of the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the technological process of the preparation method of oil-filled type insoluble sulfur that the embodiment of the present invention and comparative example provide；
Fig. 2 is the grain of raw material IS90 that the preparation method of oil-filled type insoluble sulfur that the embodiment of the present invention 20 provides uses
Diameter distribution map；
Fig. 3 be oil-filled type that the preparation method of oil-filled type insoluble sulfur that provides of the embodiment of the present invention 20 is prepared not
The grain size distribution of dissolubility sulphur.
Specific embodiment
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's all other embodiments obtained without making creative work, shall fall within the protection scope of the present invention.
The present invention provides a kind of preparation method of oil-filled type insoluble sulfur, used raw material is in this method：No
Dissolubility sulphur, filling oil and stabilizer.
Common insoluble sulfur is powdered, easily flies upward and transports inconvenience, while during rubber processing use
It is not easy to be dispersed in rubber, to environment, there are certain pollutions.Therefore it needs to carry out Oil treatment to insoluble sulfur, prevent
Only dust generates, but also insoluble sulfur and oil product are with reference to rear more readily dispersible in rubber.Insoluble sulfur belongs to unstable
Structure, if without stabilization processes, linear polymerization sulphur atom chain will be broken since both ends with faster speed, final to turn
Become the stabilization rhombic sulfur under room temperature, therefore stabilizer is added in when preparing oil-filled type insoluble sulfur, make its both ends sulphur atom
Reach rock-steady structure, to inhibit sulphur atom chain break speed, delay to soluble transformation, it is insoluble so as to improve oil-filled type
The thermostabilization of sulphur obtains quality more preferably oil-filled type insoluble sulfur.
Aforementioned stable agent include DM, PR-75 and PR-85 in it is one or more, preferably DM and PR-75 composition it is compound
The compound stabilizer of stabilizer or DM and PR-85 composition.
Wherein, DM is dibenzothiazyl disulfide；PR-75 is PR-75 type rubber disperse agent；PR-85 is PR-85 type rubber
Dispersant.
In an optional embodiment, the dosage of above-mentioned DM is the 0.2-0.9% of insoluble sulfur quality, such as can
Think but be not limited to 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%, preferably insoluble sulfur
The 0.4 of sulphur quality；The dosage of above-mentioned PR-75 is the 0.3-0.8% of insoluble sulfur quality, such as can be but be not limited to
0.3%th, 0.4%, 0.5%, 0.6%, 0.7% or 0.8%, preferably the 0.6% of insoluble sulfur quality；Above-mentioned PR-85's
Dosage is the 0.3-0.8% of insoluble sulfur quality, for example, can be but be not limited to 0.3%, 0.4%, 0.5%, 0.6%,
0.7% or 0.8%, preferably the 0.55% of insoluble sulfur quality.
In an optional embodiment, the mass fraction of insoluble sulfur is 90%- in the insoluble sulfur
100%.Improve insoluble sulfur in insoluble sulfur in raw material content can further improve oil-filled type insoluble sulfur people it is steady
It is qualitative.
In an optional embodiment, above-mentioned filling oil for example can be, but be not limited to naphthenic oil, aromatic naphtha or
Person's white oil, optionally, above-mentioned filling oil can be naphthenic oil, aromatic naphtha or white oil one or more therein；Preferably
Naphthenic oil.
Optionally, the dosage of above-mentioned filling oil is the 2%-33% of insoluble sulfur quality, such as can be, but do not limit
In 2%, 8%, 12%, 15%, 17%, 22%, 27%, 32% or 33%, preferably the 20% of insoluble sulfur quality.
The preparation method of oil-filled type insoluble sulfur provided by the invention, includes the following steps：By stabilizer and filling oil
Paste is mixed to get, then mixes above-mentioned paste with insoluble sulfur, oil-filled type insoluble sulfur is prepared.It needs
Illustrate, the preparation method of oil-filled type insoluble sulfur provided by the invention does not limit aforementioned stable agent and the mixing of filling oil
Mode is uniformly mixed, does not also limit the hybrid mode that above-mentioned paste is mixed with insoluble sulfur, is uniformly mixed.
In the present invention optionally, stabilizer is mixed to get paste with filling oil using pipeline pump；It optionally, will be in pipe
Paste in road pump, is pumped into mixing machine by pump head, is sprayed in the powder of insoluble sulfur, is uniformly mixed.
In the optional embodiment, preparation method crushes insoluble sulfur before may further include mixing
Step.Optionally, above-mentioned insoluble sulfur is crushed to 50-150 mesh, such as can be, but be not limited to 50 mesh, 70 mesh, 90 mesh,
100 mesh, 130 mesh, 140 mesh or 150 mesh, preferably 100 mesh.
In an optional embodiment, above-mentioned paste is 10-30min with above-mentioned insoluble sulfur incorporation time,
Such as can be, but be not limited to 10min, 12min, 15min, 20min, 25min or 30min preferably 15min.
The present invention provides a kind of oil-filled type insoluble sulfur, above-mentioned oil-filled type insoluble sulfur is by above-mentioned preparation method
It is prepared.
In an optional embodiment, 120 DEG C of thermal stability of above-mentioned oil-filled type insoluble sulfur is 45%-
60%.
The present invention provides a kind of application of above-mentioned oil-filled type insoluble sulfur in the vulcanization of rubber.
The present invention provides a kind of method of the vulcanization of rubber, this method uses above-mentioned oil-filled type insoluble sulfur.
It is applied in the vulcanization of rubber using oil-filled type insoluble sulfur provided by the invention, thermal stability is good, can optimize
Properties of product.
The advantageous effect further illustrated the present invention with reference to embodiment and comparative example.
The PR-75 type rubber disperses agent that the embodiment of the present invention and comparative example use believes the limited public affairs of chemical industry purchased from Qingdao benefit promise
Department, the agent of PR-85 type rubber disperses are purchased from Qingdao Yi Nuoxin Chemical Co., Ltd.s, the insoluble sulfur that the embodiment of the present invention uses
IS90 after testing, 120 DEG C, 15min thermal stability average out to 30%.The embodiment of the present invention and comparative example use other it is practical and
Equipment is commercially available conventional instrument and equipment.The preparation method of oil-filled type insoluble sulfur that the present embodiment and comparative example provide
Technological process is as shown in Figure 1.
Embodiment 1- realities embodiment 38
Embodiment 1- realities embodiment 38 provides a kind of preparation method of oil-filled type insoluble sulfur, and embodiment 1- is implemented in fact
The dosage of used raw material and raw material is as shown in table 1 in the preparation method for the oil-filled type insoluble sulfur that example 38 provides, wherein
Filling oil is naphthenic oil；Filling oily (%) is the mass percent that filling oil accounts for insoluble sulfur；DM (%) accounts for insoluble for DM
The mass percent of sulphur；PR-75 (%) is the mass percent that PR-75 accounts for insoluble sulfur；PR-85 (%) is accounted for for PR-85
The mass percent of insoluble sulfur；IS90 is the insoluble sulfur of mass fraction >=90% of insoluble sulfur；Wherein embodiment
20 grain size distributions of raw material IS90 used are as shown in Fig. 2, the preparation side for the oil-filled type insoluble sulfur that embodiment 20 provides
The grain size distribution of oil-filled type insoluble sulfur that method is prepared is as shown in Figure 3.
The raw material and original used in the preparation method of oil-filled type insoluble sulfur that 1 embodiment 1- realities embodiment 38 of table provides
The dosage of material
The processing step of the preparation method for the oil-filled type insoluble sulfur that embodiment 1- embodiments 38 provide is as follows：
(a) stabilizer will be mixed into naphthenic oil under room temperature and be mixed to get paste using pipeline pump；
(b) insoluble sulfur is ground into powder；
(c) paste in pipeline pump is pumped into mixing machine by pump head, be sprayed in the powder of insoluble sulfur, stirred
Mixing is mixed, obtains the oil-filled type insoluble sulfur of product.
Wherein, the parameter of the processing step of the preparation method of above-mentioned oil-filled type insoluble sulfur is as shown in table 2, wherein, powder
Broken mesh number represents the crushing mesh number of insoluble sulfur in step (b)；Incorporation time represents paste and insoluble sulfur in step (c)
The mixing time stirred and evenly mixed of sulphur.
The technological parameter of the preparation method for the oil-filled type insoluble sulfur that 2 embodiment 1- realities embodiment 38 of table provides
Comparative example 1- comparative examples 19
Comparative example 1- comparative examples 19 provide a kind of preparation method of oil-filled type insoluble sulfur, comparative example 1- comparative examples 19
The dosage of used raw material and raw material is as shown in table 3 in the preparation method of the oil-filled type insoluble sulfur provided, wherein filling
Oil is naphthenic oil；Filling oily (%) is the mass percent that filling oil accounts for insoluble sulfur；DM (%) accounts for insoluble sulfur for DM
Mass percent；PR-75 (%) is the mass percent that PR-75 accounts for insoluble sulfur；PR-85 (%) accounts for insoluble for PR-85
The mass percent of property sulphur；IS90 is the insoluble sulfur of mass fraction >=90% of insoluble sulfur.
Raw material and raw material used in the preparation method for the oil-filled type insoluble sulfur that table 3 comparative example 1- comparative examples 19 provide
Dosage
The processing step of the preparation method for the oil-filled type insoluble sulfur that comparative example 1- comparative examples 16 provide is as follows：
(a) stabilizer will be mixed into naphthenic oil under room temperature and be mixed to get paste using pipeline pump；
(b) insoluble sulfur is ground into powder；
(c) paste in pipeline pump is pumped into mixing machine by pump head, is sprayed in the powder of insoluble sulfur and stirs
Mixing is mixed, obtains the oil-filled type insoluble sulfur of product.
Wherein, the parameter of the processing step of the preparation method of above-mentioned oil-filled type insoluble sulfur is as shown in table 2, wherein, powder
Broken mesh number represents the crushing mesh number of insoluble sulfur in step (b)；Incorporation time represents paste and insoluble sulfur in step (c)
The mixing time stirred and evenly mixed of sulphur.
The technological parameter of the preparation method for the oil-filled type insoluble sulfur that 4 comparative example 1- comparative examples 16 of table provide
| Crush mesh number (mesh) | Incorporation time (min) | |
| Comparative example 1- comparative examples 11 | 100 | 15 |
| Comparative example 12 and comparative example 16 | 20 | 15 |
| Comparative example 13 | 200 | 15 |
| Comparative example 14 | 100 | 5 |
| Comparative example 15 | 100 | 40 |
Effect example
According to《People's Republic of China (PRC) chemical industry standard HG/T 2525-2011》The method of offer detects above-mentioned implementation
The performance of oil-filled type insoluble sulfur that the preparation method of oil-filled type insoluble sulfur that example and comparative example provide is prepared, knot
Fruit is as shown in table 5：
The performance of 5 oil-filled type insoluble sulfur of table
The preparation method of oil-filled type insoluble sulfur that embodiment 1- realities embodiment 38 provides it can be seen from upper table data
The oil-filled type insoluble sulfur prepared has higher 120 DEG C, the thermal stability of 15min.
Wherein, it is compared by embodiment 1- embodiments 15 and embodiment 20- embodiments 25 it can be seen that using compound stabilizer
Better than using single stable agent；Embodiment 1-25 and comparative example 1-9 comparisons are as can be seen that the dosage of suitable stabilizer can
To improve the thermal stability of oil-filled type insoluble sulfur, what wherein embodiment 20 and embodiment 25 provided meets stabilizer and its makes
Dosage is due to other embodiment；And it can be seen from embodiment 26 when compound stabilizer simultaneously using DM, PR-75 and
There is no the formula scheme of compound stabilizer provided due to embodiment 20 and embodiment 25 during PR-85, it is in and is produced into
This consideration, embodiment 20 and embodiment 25 are a kind of preferred schemes.
Wherein, by embodiment 27- embodiments 30 and comparative example 10- comparative examples 11 compare it is found that the dosage of naphthenic oil also can
The thermal stability of oil-filled type insoluble sulfur is influenced, in the technical program, fills the cycloalkanes of the quality 20% of insoluble sulfur
Oil can make oil-filled type insoluble sulfur have higher thermal stability.
Wherein, by embodiment 31- realities embodiment 38 and comparative example 12- comparative examples 16 compare it can be seen from the present invention provide
The technological parameter of preparation method of oil-filled type insoluble sulfur can make the oil-filled type insoluble sulfur being prepared by optimization
120 DEG C of sulphur, the thermal stability of 15min significantly improves.
Wherein, by Fig. 2 and Fig. 3 comparisons it is found that the preparation method of oil-filled type insoluble sulfur that embodiment 20 provides, into one
Step integrates the granularity of insoluble sulfur, and the particle size distribution of insoluble sulfur is made further to concentrate, improves dispersibility, optimizes
Product performance.
In conclusion optimization of the preparation method of oil-filled type insoluble sulfur provided by the invention by raw material and technique
Make its 120 DEG C of oil-filled type insoluble sulfur be prepared, the thermal stability of 15min significantly improves.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe is described in detail the present invention with reference to foregoing embodiments, it will be understood by those of ordinary skill in the art that：Its according to
Can so modify to the technical solution recorded in foregoing embodiments either to which part or all technical features into
Row equivalent replacement；And these modifications or replacement, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of preparation method of oil-filled type insoluble sulfur, which is characterized in that the preparation method includes the following steps：It will be steady
Determine agent and be mixed to get paste with filling oil, then gained paste with insoluble sulfur is mixed, oil-filled type is prepared not
Dissolubility sulphur；
Wherein, the stabilizer includes dibenzothiazyl disulfide, PR-75 type rubber disperse agent and PR-85 type rubber disperse agent
In it is one or more；
Preferably, the stabilizer is formed for dibenzothiazyl disulfide and the agent of PR-75 type rubber disperses compound stabilizer or
The compound stabilizer of dibenzothiazyl disulfide and PR-85 type rubber disperses agent composition.
2. preparation method according to claim 1, which is characterized in that the dosage of the dibenzothiazyl disulfide is insoluble
Property sulphur quality 0.2%-0.9%, the dosage of the PR-75 types rubber disperse agent is the 0.3%- of insoluble sulfur quality
0.8%, the dosage of the PR-85 types rubber disperse agent is the 0.3%-0.8% of insoluble sulfur quality；
Preferably, the dosage of the dibenzothiazyl disulfide is the 0.3%-0.6%, the PR-75 of insoluble sulfur quality
The dosage of type rubber disperse agent is the 0.5%-0.7% of insoluble sulfur quality, and the dosage of the PR-85 types rubber disperse agent is
The 0.5%-0.7% of insoluble sulfur quality；
It is further preferred that the dosage of the dibenzothiazyl disulfide is the 0.4% of insoluble sulfur quality, the PR-75
The dosage of type rubber disperse agent is the 0.6% of insoluble sulfur quality, and the dosage of the PR-85 types rubber disperse agent is insoluble
The 0.55% of sulphur quality.
3. preparation method according to claim 1, which is characterized in that the quality of insoluble sulfur point in the insoluble sulfur
Number is 90%-100%.
4. preparation method according to claim 1, which is characterized in that the dosage of the filling oil is insoluble sulfur quality
2%-33%；
Preferably, the dosage of the filling oil is the 10%-30% of insoluble sulfur quality；
It is further preferred that the dosage of the filling oil is the 20% of insoluble sulfur quality.
5. preparation method according to claim 1, which is characterized in that before the preparation method may further include mixing
The step of insoluble sulfur is crushed；
Preferably, it is that insoluble sulfur is crushed to 50-150 mesh.
6. preparation method according to claim 1, which is characterized in that when the paste is mixed with the insoluble sulfur
Between be 10-30min.
7. a kind of oil-filled type insoluble sulfur, which is characterized in that the oil-filled type insoluble sulfur is by any one of claim 1-6
The preparation method is prepared.
8. oil-filled type insoluble sulfur according to claim 7, which is characterized in that the oil-filled type insoluble sulfur
120 DEG C of thermal stability is 45%-60%.
9. application of the oil-filled type insoluble sulfur in the vulcanization of rubber described in claim 7 or 8.
A kind of 10. method of the vulcanization of rubber, which is characterized in that in the method using the oil-filled type described in claim 7 or 8 not
Dissolubility sulphur.
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| CN104843651A (en) * | 2014-02-18 | 2015-08-19 | 中国石油化工股份有限公司 | Production process for preparing insoluble sulphur through low temperature method |
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| CN1462721A (en) * | 2002-05-30 | 2003-12-24 | 中国科学院大连化学物理研究所 | Method for preparing high quality insoluble sulphur |
| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| CN104843651A (en) * | 2014-02-18 | 2015-08-19 | 中国石油化工股份有限公司 | Production process for preparing insoluble sulphur through low temperature method |
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