CN108329700A - A kind of production method of polymolecularity high stability insoluble sulfur - Google Patents
A kind of production method of polymolecularity high stability insoluble sulfur Download PDFInfo
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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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/12—Insoluble sulfur (mu-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
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a kind of production methods of polymolecularity high stability insoluble sulfur, belong to sulphur into production technical field.The production method of the polymolecularity high stability insoluble sulfur of the present invention, using liquid-state sulfur as raw material, middle grade insoluble sulphur is prepared using gasification chilling method, then grade insoluble sulphur in this extracted successively, dried, is sieved and Oil treatment obtains the insoluble sulfur product, suitable stabilizer is added thereto when wherein grade insoluble sulphur is dried after extraction in gained, and suitable fatty alcohol polyoxyethylene ether is added when Oil treatment thereto, aforementioned stable agent is formulated by ammonium persulfate, sodium ethyl xanthate and iodine.Production method using the present invention can effectively improve the thermal stability and dispersion performance of gained insoluble sulfur, to ensure its application effect.
Description
Technical field
The invention belongs to sulfur cream technical fields, insoluble more specifically to a kind of polymolecularity high stability
The production method of sulphur.
Background technology
Insoluble sulfur is also known as elastic sulfur or polymerised sulphur, by a large amount of sulphur atoms by the linear polymeric that is polymerized,
Relative molecular mass is a kind of nontoxic, flammable yellow powder, gains the name because it is insoluble in carbon disulfide, it is up to tens thousand of
The allotrope of the high polymeric species of common sulphur and macromolecule modified kind.Currently, the insoluble sulfur overwhelming majority is used for
Rubber industry, advanced accelerating agent and vulcanizing agent as a kind of rubber industry are widely used in tire and other rubber are compound
In the manufacturing of product, the rubber such as the carcass sizing material of tire, buffering sizing material, white sidewall rubber and tyre retreading, sebific duct, adhesive tape with
In the sizing material of framework material bonding, it can also be used in the sizing material of the rubber products such as cable, rubber roller, oil sealing, rubber overshoes, while also apply
In the big light-colour rubber product of sulfur consumption.
With the improvement of road traffic and the development of auto industry, the car speed of continuous improvement proposes higher to tire
It is required that radial will replace Conventi onal bias tyre, become the inexorable trend of tire industry development, the head as radial
Vulcanizer, the demand of insoluble sulfur is selected to increase year by year therewith.It is improved by years of researches, although China is insoluble
Property sulphur technique achieve significant progress, production scale is gradually expanded, and properties of product are gradually increased, but and external performance it is excellent
Different product is compared, and does not still have the thermal stability and dispersion performance of competitiveness, especially insoluble sulfur.Thermal stability
With dispersion performance it may be said that play the role of to the application of insoluble sulfur product it is vital, wherein since insoluble sulfur is
A kind of metastable state substance, stability can be increased with temperature and is deteriorated when exclusive use, and content can with longer storage duration and by
Step reduces, and dispersion performance then directly influences the mixing uniformity of sulphur and sizing material, therefore thermal stability and dispersion performance
Quality directly has large effect to rubber product, such as performance of wheel tyre and service life.Therefore, production how is improved
The thermal stability and dispersion performance of gained insoluble sulfur just have great importance for its application in rubber product.
Currently, the thermal stability and the relatively poor problem of dispersion performance, China for insoluble sulfur are largely insoluble
Property sulfur cream producer be typically by adding certain additive during sulfur cream, such as heat stabilizer and surface-active
Agent improves its thermal stability and dispersion performance.Such as, the application case that Chinese Patent Application No. is 200810141306.3 discloses
A kind of production technology of rubber insoluble sulfur, this application is using common sulphur as raw material, under conditions of 250 DEG C -350 DEG C
Melting, then in 600 DEG C of -850 DEG C of gasifications, then quenching lacing film, dry, pulverize, and extraction, addition is by antioxygen after extraction
Agent, Isobutylxanthic acid and styrene composition compound stabilizer, the mass ratio that wherein antioxidant, Isobutylxanthic acid and alkene are blamed is
1-2:1-3:0.5-2.This application during sulfur cream by adding above-mentioned compound stabilizer, to a certain extent
The thermal stability of gained sulfur product can be improved, but the thermal stability of gained sulfur product still needs to be further increased, and its
Heat-resistant stability degradation phenomena also easy to happen during long-term storage, to influence it subsequently in the rubber products such as tire
Performance.
For another example, Chinese Patent Application No. is 2015103967 36.X, and the applying date is：On 07 08th, 2015, innovation and creation
It is entitled：A method of improving dispersity of insoluble sulfur, this application selection fusing point or softening point have at 40-100 DEG C
Machine object is as dispersive material, and before insoluble sulfur is oil-filled, heating makes dispersive material keep molten state, then by melting
Dispersive material is uniformly sprayed onto insoluble sulfur surface with mist, carries out filling out envelope to the micropore on insoluble sulfur surface, waits disperseing
Property material carries out oil-filled again after being sufficiently mixed with insoluble sulfur.This application by by fusing point or softening point at 40-100 DEG C
Organic matter is added in insoluble sulfur using molten state as dispersant, then carries out Oil treatment again, to a certain degree
On can improve the dispersion performance of gained insoluble sulfur product, but its operation is complex, needs additionally to increase by a procedure.
Invention content
1. technical problems to be solved by the inivention
It is an object of the invention to overcome to use the thermal stability of insoluble sulfur obtained by domestic prior art production and divide
The relatively poor deficiency of property is dissipated, a kind of production method of polymolecularity high stability insoluble sulfur is provided.Using the present invention
Production method can effectively improve gained insoluble sulfur thermal stability and dispersion performance, to ensure its application effect.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention is：
A kind of production method of polymolecularity high stability insoluble sulfur of the present invention is adopted using liquid-state sulfur as raw material
Middle grade insoluble sulphur is prepared with gasification-chilling method, then grade insoluble sulphur in this is extracted successively, is done
Dry, sieving and Oil treatment obtain the insoluble sulfur product, wherein grade insoluble sulphur carries out after extraction in gained
Suitable stabilizer is added when drying process thereto, and adds suitable aliphatic alcohol polyethenoxy when Oil treatment thereto
Ether, aforementioned stable agent are formulated by ammonium persulfate, sodium ethyl xanthate and iodine.
Further, the additive amount of the fatty alcohol polyoxyethylene ether is the 0.4- of gained insoluble sulfur finished product gross weight
0.6%.
Further, the mass ratio of ammonium persulfate and sodium ethyl xanthate is 3 in the stabilizer：(4-5), ammonium persulfate
The mass ratio of the mother liquor and iodine that are formed with sodium ethyl xanthate is (119-121)：1.
Further, the additive amount of the stabilizer is the 2%-3% of gained insoluble sulfur product quality.
Further, the preparation process of the stabilizer is：By ammonium persulfate and sodium ethyl xanthate according to quality score
It is not added to the water, with sodium ethyl xanthate reacted rear and water precipitated and separated occurs for ammonium persulfate, through detaching up to ammonium persulfate
With the stabilizer mother liquor of sodium ethyl xanthate composition, iodine is then added into stabilizer mother liquor and is uniformly mixed up to stabilizer.
Further, it is the middle product after extracting when grade insoluble sulphur is dried after extraction in gained
Position insoluble sulfur is uniformly mixed with stabilizer to be placed in dry pot, so that product temperature is risen to 60 by 15 DEG C using hot water heating
It DEG C is dried.
Further, the extract liquor selects CS2, the described sieving carried out using the sieve of 100-150 mesh.
Further, the mixing quality percentage of insoluble sulfur semi-finished product and rubber oil is distinguished when the Oil treatment
For (79-81) %, (19-21) %.
Further, the rubber oil is naphthenic oil.
Further, H is added in the liquid-state sulfur raw material2S, H2The additive amount of S is liquid-state sulfur quality
0.000001-3%.
3. advantageous effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result：
(1) production method of a kind of polymolecularity high stability insoluble sulfur of the invention, wherein middle grade insoluble
It adds when sulphur is dried after extraction and suitable to be formulated by ammonium persulfate, sodium ethyl xanthate and iodine thereto
Compound stabilizer, and suitable fatty alcohol polyoxyethylene ether is added when Oil treatment thereto, so as to effectively improve gained
The thermal stability and dispersion performance of insoluble sulfur product, and then ensure application effect of the insoluble sulfur product in rubber.
In addition, the compatibility between stabilizer and surfactant and insoluble sulfur selected by the present invention is preferable, sulphur will not be produced
The physicochemical property of product causes harmful effect.
(2) production method of a kind of polymolecularity high stability insoluble sulfur of the invention, by each in stabilizer
The additive amount of the proportioning of component, the additive amount of the stabilizer and fatty alcohol polyoxyethylene ether optimizes, on the one hand
The thermal stability and dispersion performance that can ensure gained insoluble sulfur product reach best fit, on the other hand can also be effective
Prevent additive from adding the grade of multipair products obtained therefrom and the influence of other physicochemical properties.
(3) production method of a kind of polymolecularity high stability insoluble sulfur of the invention, inventor pass through a large amount of real
It tests, stabilizer is added in selection in dry treatment process, and is strictly controlled the temperature of drying process, to have
Effect ensures giving full play to for stabilizer function, while can also reduce the influence being dried to products obtained therefrom sulfur grade, prevents
The sulfur content of product declines after drying process.
(4) production method of a kind of polymolecularity high stability insoluble sulfur of the invention, by into liquid material
Add suitable H2S is conducive to the stability for further increasing products obtained therefrom so as to effectively reduce the vigorous degree of raw material.
Specific implementation mode
To further appreciate that present disclosure, in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of production method of the polymolecularity high stability insoluble sulfur of the present embodiment, using liquid-state sulfur as raw material,
Middle grade insoluble sulphur is prepared using gasification-chilling method, then extracted grade insoluble sulphur in this successively,
Dry, sieving and Oil treatment obtain the insoluble sulfur product, wherein grade insoluble sulphur is laggard through extracting in gained
Row adds suitable stabilizer thereto when being dried, and adds suitable aliphatic alcohol polyethenoxy when Oil treatment thereto
Ether, aforementioned stable agent are formulated by ammonium persulfate, sodium ethyl xanthate and iodine.Specifically, over cure in the stabilizer of the present embodiment
The mass ratio of sour ammonium and sodium ethyl xanthate is 3：4, the mass ratio of mother liquor and iodine that ammonium persulfate is formed with sodium ethyl xanthate is
119：1, and 2% that the additive amount of stabilizer is gained insoluble sulfur product quality, the additive amount of fatty alcohol polyoxyethylene ether
It is the 0.6% of gained insoluble sulfur finished product gross weight.The preparation process of aforementioned stable agent is：By ammonium persulfate and sodium ethyl xanthate
It is added separately in water according to mass ratio, with sodium ethyl xanthate reacted rear and water precipitated and separated occurs for ammonium persulfate, through separation
Up to the stabilizer mother liquor of ammonium persulfate and sodium ethyl xanthate composition, iodine is then added into stabilizer mother liquor and is uniformly mixed i.e.
Obtain stabilizer.
In the prior art when producing insoluble sulfur product, be usually all by some additives, such as heat stabilizer and
The addition of surfactant improves the thermal stability and dispersion performance of product.Currently, in the prior art mainly by adding
Add iodine or styrenes to improve the thermal stability of insoluble sulfur, but its effect is still to be improved, and adds existing normal
When with stabilizer, with the extension of product storage time, the IS contents of product can gradually reduce, when being used to influence product
Quality.Meanwhile although surfactant used in existing insoluble sulfur production can improve point of the product in sizing material
Performance is dissipated, but its effect still needs to be further increased.In addition, improving sulphur by the addition of surfactant in the prior art
Its dispersion performance is usually only considered when the dispersion performance of product, and other physicochemical properties of products obtained therefrom are then not concerned with.And
Present inventor has found that current existing conventional surfactant would generally cause to produce to a certain extent in experimental study
Moral character especially can generate the thermal stability of product certain influence with the decline of quality, insoluble so as to cause gained
The comprehensive performance of sulfur product is still difficult to the application demand met in rubber product.
Based on problem above, the present inventor has carried out long-term a large amount of experimental study, in conjunction with the property of sulfur product
Matter finally found that, by adding suitable compound stabilizer being formulated by ammonium persulfate, sodium ethyl xanthate and iodine, and fill
Suitable fatty alcohol polyoxyethylene ether is added when oil processing thereto, so as to effectively improve gained insoluble sulfur product
Thermal stability and dispersion performance, and the addition of fatty alcohol polyoxyethylene ether substantially will not be to other physicochemical properties of product, especially
It is that thermal stability has an impact, and to make to be coordinated well therebetween, and then can ensure insoluble sulfur product
Application effect in rubber.
Comparative example 1
The difference of this comparative example and embodiment 1 essentially consists in：It is any using not added in Oil feeding process in this comparative example
Antistatic agent.
Comparative example 2
The difference of this comparative example and embodiment 1 essentially consists in：It is used in this comparative example and adds fatty alcohol in Oil feeding process
Ether phosphoric acid fat sylvite replaces fatty alcohol polyoxyethylene ether.
Comparative example 3
The difference of this comparative example and embodiment 1 essentially consists in：It is used in this comparative example and adds fatty alcohol in Oil feeding process
Ether phosphoric acid fat sylvite and the mixture of fatty alcohol polyoxyethylene ether replace fatty alcohol polyoxyethylene ether.
Inventor has found by lot of experiments, relative to other added in existing insoluble sulfur production technology
Antistatic agent can effectively improve point of products obtained therefrom using the antistatic agent in embodiment 1 and comparative example 2 and comparative example 3
Performance is dissipated, is found through oil-filled experiment, three occurs without electrostatic phenomenon, and antistatic effect is preferable.By the present embodiment and comparison
Example 2 and comparative example 3, which produce products obtained therefrom and be added to, to be taken difference to be detected the sulphur contained in sizing material to carry out its inspection in sizing material
It surveys sulphur and is uniformly dispersed situation inside sizing material to verify dispersibility, as a result as shown in table 1 below, this reality it can be seen from table
It applies dispersion performance of the production gained sulphur in rubber product in example and is better than comparative example 1-3.
The sulfur content of difference in 1 embodiment 1 of table and comparative example 1-3 products obtained therefroms
| Difference | Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| 1 | 1.1728 | 1.1726 | 1.1757 | 1.1694 |
| 2 | 1.1727 | 1.1494 | 1.1720 | 1.1715 |
| 3 | 1.1657 | 1.1487 | 1.1557 | 1.1859 |
| 4 | 1.1704 | 1.1457 | 1.1428 | 1.1783 |
| 5 | 1.1724 | 1.1721 | 1.1756 | 1.1656 |
| 6 | 1.1704 | 1.1624 | 1.1572 | 1.1652 |
In addition, inventor has found in the course of the research, products obtained therefrom will be produced in embodiment 1 and comparative example 2 and comparative example 3
Physicochemical test test, as a result as shown in table 2 below, the heat of product in comparative example it can be seen from table 2 and comparative example 3 are carried out respectively
Stability is a greater impact, and declines seriously, and the thermal stability of products obtained therefrom and other physicochemical properties are basic in the present embodiment
It is upper unaffected, it remains to meet requirement.
The physicochemical property test result of 2 embodiment 1 of table and comparative example 1-3 products obtained therefroms
Comparative example 4
The difference of this comparative example and embodiment 1 essentially consists in：Stabilizer used is iodine in this comparative example.
Comparative example 5
The difference of this comparative example and embodiment 1 essentially consists in：Stabilizer used is α-methylstyrene in this comparative example.
Comparative example 6
The difference of this comparative example and embodiment 1 essentially consists in：Stabilizer used is ammonium persulfate and ethyl in this comparative example
The mixture of sodium xanthate.
The thermal stability that gained GOOD TASTE insoluble sulfur product is prepared in embodiment 1 and comparative example 4-6 is carried out respectively
Test, the results showed that, when using α-methylstyrene as product stabilizer, since α-methylstyrene volatilization is serious, lead
Cause the thermal stability of product relatively poor, and more serious, its thermostabilization at 105 DEG C × 15min after one month of degenerating
Property i.e. be down to 73% or less；And works as and use the mixture of halogen iodine and ammonium persulfate and sodium ethyl xanthate as product stabilizer
When, the thermal stability of product effectively improves relative to α-methylstyrene, but product its thermostabilization during storage
Property significant degradation can occur, wherein using iodine when shelf-life can only control within 3 months, use ammonium persulfate and ethyl sodium
The shelf-life of product was close to 9 months when the mixture of xanthate is as stabilizer.And it is steady when using the mixture of the present embodiment to be used as
Determine to be not only able to effectively improve when agent the thermal stability of product, and thermal stability of product during follow-up storage degenerate compared with
Few, shelf life of products is longer, and the thermal stability of product is still substantially without occurring degradation phenomena after storing 1 year, to be conducive to
Its application effect subsequently in rubber product.
Embodiment 2
A kind of production method of polymolecularity high stability insoluble sulfur of the present embodiment, the difference to embodiment 1
It essentially consists in：The mass ratio of ammonium persulfate and sodium ethyl xanthate is 3 in the stabilizer of the present embodiment：5, ammonium persulfate and ethyl sodium
The mass ratio of mother liquor and iodine that xanthate is formed is 121：1, and the additive amount of stabilizer is gained insoluble sulfur product quality
3%, the additive amount of fatty alcohol polyoxyethylene ether is the 0.4% of gained insoluble sulfur finished product gross weight.The extraction of the present embodiment
Liquid selects CS2, be when being dried after extraction middle grade insoluble sulphur after extracting with stabilizer after mixing
It is placed in dry pot, so that product temperature is risen to 60 DEG C by 15 DEG C using hot water heating and be dried, then by the product after drying
It is sieved using the sieve of 100-150 mesh, obtains insoluble sulfur semi-finished product, finally by the insoluble sulfur semi-finished product and rubber
Glue oil, which is uniformly mixed, carries out Oil treatment, the mixing quality percentage of insoluble sulfur semi-finished product and rubber oil is respectively 79%,
21%.
Inventor adds stabilizer by many experiments, selection in dry treatment process, and to the temperature of drying process
It is strictly controlled, to which giving full play to for stabilizer function can either be effectively ensured, while drying process pair can also be reduced
The influence of products obtained therefrom sulfur grade prevents the sulfur content of the product after drying process from declining.The heat of the present embodiment products obtained therefrom is steady
Qualitative and dispersion performance is closer to 1 products obtained therefrom of embodiment.
Embodiment 3
A kind of production method of polymolecularity high stability insoluble sulfur of the present embodiment, the difference to embodiment 2
It essentially consists in：The mass ratio of ammonium persulfate and sodium ethyl xanthate is 3 in the stabilizer of the present embodiment：4, ammonium persulfate and ethyl sodium
The mass ratio of mother liquor and iodine that xanthate is formed is 120：1, and the additive amount of stabilizer is gained insoluble sulfur product quality
3%, the additive amount of fatty alcohol polyoxyethylene ether is the 0.5% of gained insoluble sulfur finished product gross weight.It should in the present embodiment
When insoluble sulfur semi-finished product mix progress Oil treatment with rubber oil, the mixing quality of insoluble sulfur semi-finished product and rubber oil
Percentage is respectively 80%, 20%.The thermal stability and dispersion performance of the present embodiment products obtained therefrom and 1 products obtained therefrom of embodiment compared with
It is close.
Embodiment 4
A kind of production method of polymolecularity high stability insoluble sulfur of the present embodiment, the difference to embodiment 3
It essentially consists in：The mass ratio of ammonium persulfate and sodium ethyl xanthate is 3 in the stabilizer of the present embodiment：4.5, ammonium persulfate and ethyl
The mass ratio of mother liquor and iodine that sodium xanthate is formed is 120：1, and the additive amount of stabilizer is gained insoluble sulfur product matter
The 2.5% of amount, the additive amount of fatty alcohol polyoxyethylene ether are the 0.5% of gained insoluble sulfur finished product gross weight.In the present embodiment
The insoluble sulfur semi-finished product are mixed with rubber oil when carrying out Oil treatment, the mixing of insoluble sulfur semi-finished product and rubber oil
Mass percent is respectively 81%, 19%, and is added into liquid-state sulfur raw material when grade insoluble sulphur semi-finished product in preparation
The H of liquid-state sulfur total amount 0.07%2S is conducive to further increase products obtained therefrom so as to effectively reduce the vigorous degree of raw material
Stability.The thermal stability and dispersion performance of the present embodiment products obtained therefrom are closer to 1 products obtained therefrom of embodiment.
Embodiment 5
A kind of production method of polymolecularity high stability insoluble sulfur of the present embodiment, the difference with embodiment 4
It essentially consists in：The rubber oil of the present embodiment is naphthenic oil, and liquid-state sulfur used in grade insoluble sulphur semi-finished product is former in preparation
H in material2The additive amount of S is the 1.2% of liquid-state sulfur quality.
Embodiment 6
A kind of production method of polymolecularity high stability insoluble sulfur of the present embodiment, the difference with embodiment 5
It essentially consists in：H in liquid-state sulfur raw material used in grade insoluble sulphur semi-finished product in being prepared in the present embodiment2The additive amount of S is
The 3% of liquid-state sulfur quality.The thermal stability and dispersion performance of the present embodiment products obtained therefrom more connect with 1 products obtained therefrom of embodiment
Closely.
Claims (10)
1. a kind of production method of polymolecularity high stability insoluble sulfur, it is characterised in that：Using liquid-state sulfur as raw material, adopt
Middle grade insoluble sulphur is prepared with gasification-chilling method, then grade insoluble sulphur in this is extracted successively, is done
Dry, sieving and Oil treatment obtain the insoluble sulfur product, wherein grade insoluble sulphur carries out after extraction in gained
Suitable stabilizer is added when drying process thereto, and adds suitable aliphatic alcohol polyethenoxy when Oil treatment thereto
Ether, aforementioned stable agent are formulated by ammonium persulfate, sodium ethyl xanthate and iodine.
2. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 1, it is characterised in that：
The additive amount of the fatty alcohol polyoxyethylene ether is the 0.4-0.6% of gained insoluble sulfur finished product gross weight.
3. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 1, it is characterised in that：
The mass ratio of ammonium persulfate and sodium ethyl xanthate is 3 in the stabilizer：(4-5), ammonium persulfate are formed with sodium ethyl xanthate
The mass ratio of mother liquor and iodine is (119-121)：1.
4. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 3, it is characterised in that：
The additive amount of the stabilizer is the 2%-3% of gained insoluble sulfur product quality.
5. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 3 or 4, feature exist
In：The preparation process of the stabilizer is：Ammonium persulfate and sodium ethyl xanthate are added separately to according to mass ratio in water, over cure
With sodium ethyl xanthate reacted rear and water precipitated and separated occurs for sour ammonium, through detaching up to ammonium persulfate and sodium ethyl xanthate composition
Then iodine is added into stabilizer mother liquor and is uniformly mixed up to stabilizer for stabilizer mother liquor.
6. a kind of production method of polymolecularity high stability insoluble sulfur according to any one of claim 1-4,
It is characterized in that：It is the middle grade insoluble after extracting when grade insoluble sulphur is dried after extraction in gained
Sulphur is uniformly mixed with stabilizer and is placed in dry pot, so that product temperature is risen to 60 DEG C by 15 DEG C using hot water heating and is done
It is dry.
7. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 6, it is characterised in that：
The extract liquor selects CS2, the described sieving carried out using the sieve of 100-150 mesh.
8. a kind of production method of polymolecularity high stability insoluble sulfur according to any one of claim 1-4,
It is characterized in that：The mixing quality percentage of insoluble sulfur semi-finished product and rubber oil is respectively (79- when the Oil treatment
81) %, (19-21) %.
9. a kind of production method of polymolecularity high stability insoluble sulfur according to claim 8, it is characterised in that：
The rubber oil is naphthenic oil.
10. a kind of production method of polymolecularity high stability insoluble sulfur according to any one of claim 1-4,
It is characterized in that：H is added in the liquid-state sulfur raw material2S, H2The additive amount of S is the 0.000001- of liquid-state sulfur quality
3%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146424A (en) * | 1996-08-08 | 1997-04-02 | 赵水斌 | Insoluble sulphur preparation method and production device |
| CN101712010A (en) * | 2009-11-27 | 2010-05-26 | 江苏宏泰橡胶助剂有限公司 | Method for improving dispersity of insoluble sulfur |
| CN102398896A (en) * | 2011-09-30 | 2012-04-04 | 河南省开仑化工有限责任公司 | New production technology of insoluble sulfur for rubber use |
| CN102633234A (en) * | 2012-04-06 | 2012-08-15 | 中国石油大学(华东) | Insoluble sulfur stabilizing agent and preparation method thereof |
-
2018
- 2018-04-28 CN CN201810399141.3A patent/CN108329700B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146424A (en) * | 1996-08-08 | 1997-04-02 | 赵水斌 | Insoluble sulphur preparation method and production device |
| CN101712010A (en) * | 2009-11-27 | 2010-05-26 | 江苏宏泰橡胶助剂有限公司 | Method for improving dispersity of insoluble sulfur |
| CN102398896A (en) * | 2011-09-30 | 2012-04-04 | 河南省开仑化工有限责任公司 | New production technology of insoluble sulfur for rubber use |
| CN102633234A (en) * | 2012-04-06 | 2012-08-15 | 中国石油大学(华东) | Insoluble sulfur stabilizing agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王柳英: "不溶性硫磺的制备及性能研究", 《中国优秀硕士论文全文数据库 工程科技I辑》 * |
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| CN108329700B (en) | 2020-05-19 |
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