CN108129693B - Oil-extended insoluble sulfur and preparation method and application thereof - Google Patents
Oil-extended insoluble sulfur and preparation method and application thereof Download PDFInfo
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- CN108129693B CN108129693B CN201711415263.9A CN201711415263A CN108129693B CN 108129693 B CN108129693 B CN 108129693B CN 201711415263 A CN201711415263 A CN 201711415263A CN 108129693 B CN108129693 B CN 108129693B
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- 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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- C08L21/00—Compositions of unspecified rubbers
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- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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Abstract
The invention provides oil-filled insoluble sulfur and a preparation method and application thereof, and relates to the technical field of vulcanizing agent preparation. According to the preparation method of the oil-filled insoluble sulfur, the stabilizer and the filling oil are mixed to obtain the paste, and then the paste and the insoluble sulfur are mixed to obtain the oil-filled insoluble sulfur, so that the oil-filled insoluble sulfur has good thermal stability and dispersibility, the product use performance is optimized, the technical problems of poor quality of the preparation method of the oil-filled insoluble sulfur and the prepared oil-filled insoluble sulfur in the prior art are solved, the oil-filled insoluble sulfur reaches the standards of the same industry in foreign countries, and the monopoly of the foreign countries is hopefully broken.
Description
Technical Field
The invention relates to the technical field of vulcanizing agent preparation, in particular to oil-extended insoluble sulfur and a preparation method and application thereof.
Background
Sulfur is an important vulcanizing agent for rubber, and common sulfur used in rubber formulations is stable orthorhombic crystal which is soluble in rubber hydrocarbon at processing and vulcanizing temperatures, but as the rubber cools during standing, the sulfur rapidly diffuses to the surface of the rubber and crystallizes, causing surface sulfur spraying. Such sulfur spraying can affect the processability and usability of the compound, such as adhesion between cords and the like.
Insoluble Sulfur (IS), a chain polymer of Sulfur, IS so called because it IS Insoluble in carbon disulfide and rubber hydrocarbon. The insoluble sulfur is mainly used as a high-grade accelerator and a vulcanizing agent in the rubber industry and is widely applied to the production and the manufacture of tires and other rubber composite products, such as tire body rubber compounds, buffer rubber compounds, white sidewall rubber, retreading, rubber tubes, adhesive tapes and other rubber and framework material bonding rubber compounds of the tires, and can also be applied to rubber compounds of rubber products such as cables, rubber rollers, oil seals, rubber shoes and the like, and also applied to light-colored rubber products with large sulfur consumption. Because the insoluble sulfur can ensure that meridian lines, steel wires and rubber are more firmly adhered, the glue stock is effectively prevented from blooming, and the heat resistance and the wear resistance of the tire are improved. Therefore, insoluble sulfur is an essential important raw material in tire production. The insoluble sulfur is insoluble in rubber due to the characteristic of linear macromolecules, cannot migrate to the surface of rubber materials, cannot generate sulfur spraying, can also improve the white viscosity of the rubber materials, improves the bonding strength between layers of rubber products, can shorten the vulcanization period, has good wear resistance, is improved by 30-50 percent compared with a common tire, and has the service life 1.5 times longer than that of the common tire.
Insoluble sulphur products are generally treated to be oil extended. However, the quality index can not meet the use requirement for a long time in China, particularly the stability at 120 ℃, the domestic market of oil-filled insoluble sulfur is monopolized by foreign countries, the bottleneck is brought to the development of the domestic tire industry, and the demand of the insoluble sulfur is greatly driven by the rapid growth of radial tires along with the improvement of road traffic and the development of automobile processes. The product is heavily dependent on import. Therefore, a preparation method for preparing oil-extended insoluble sulfur having good thermal stability and an oil-extended insoluble sulfur having good thermal stability are in great demand in the market at present.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of oil-extended insoluble sulfur, which solves the technical problem of poor thermal stability of the oil-extended insoluble sulfur prepared by the preparation method of the oil-extended insoluble sulfur in the prior art.
The second purpose of the invention is to provide oil-extended insoluble sulfur, which solves the technical problem of poor thermal stability of the oil-extended insoluble sulfur prepared by the prior art.
The third purpose of the invention is to provide the application of the oil-filled insoluble sulfur in rubber vulcanization, which solves the technical problem that the prior art lacks an application of the oil-filled insoluble sulfur which has good thermal stability in rubber vulcanization.
The fourth purpose of the invention is to provide a rubber vulcanization method, which uses the oil-filled insoluble sulfur and solves the technical problem that the oil-filled insoluble sulfur with good thermal stability is lacked in the rubber vulcanization method in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of oil-extended insoluble sulfur comprises the following steps: mixing the stabilizer with filling oil to obtain paste, and mixing the paste with insoluble sulfur to obtain oil-filled insoluble sulfur;
wherein the stabilizer comprises one or more of dibenzothiazyl disulfide, a rubber dispersant of PR-75 type and a rubber dispersant of PR-85 type;
preferably, the stabilizer is a composite stabilizer consisting of dibenzothiazyl disulfide and a PR-75 type rubber dispersant or a composite stabilizer consisting of dibenzothiazyl disulfide and a PR-85 type rubber dispersant.
Further, the dosage of the dibenzothiazyl disulfide is 0.2-0.9% of the mass of the insoluble sulfur, the dosage of the PR-75 type rubber dispersant is 0.3-0.8% of the mass of the insoluble sulfur, and the dosage of the PR-85 type rubber dispersant is 0.3-0.8% of the mass of the insoluble sulfur;
preferably, the amount of the dibenzothiazyl disulfide is 0.3-0.6% of the mass of the insoluble sulfur, the amount of the PR-75 type rubber dispersant is 0.5-0.7% of the mass of the insoluble sulfur, and the amount of the PR-85 type rubber dispersant is 0.5-0.7% of the mass of the insoluble sulfur;
more preferably, the amount of the dibenzothiazyl disulfide is 0.4 percent of the mass of the insoluble sulfur, the amount of the PR-75 type rubber dispersant is 0.6 percent of the mass of the insoluble sulfur, and the amount of the PR-85 type rubber dispersant is 0.55 percent of the mass of the insoluble sulfur.
Further, the mass fraction of insoluble sulfur in the insoluble sulfur is 90-100%.
Further, the using amount of the filling oil is 2-33% of the mass of the insoluble sulfur;
preferably, the filling oil is used in an amount of 10% -30% of the mass of the insoluble sulfur;
further preferably, the extender oil is used in an amount of 20% by mass of the insoluble sulphur.
Further, the preparation method further comprises the step of crushing the insoluble sulfur before mixing;
preferably, the insoluble sulfur is pulverized to 50-150 mesh.
Further, the paste and the insoluble sulfur are mixed for 10-30 min.
An oil-extended insoluble sulfur, which is prepared by the preparation method.
Further, the heat stability of the oil-extended insoluble sulfur at 120 ℃ is 45-60%.
An application of the oil-extended insoluble sulfur in rubber vulcanization.
A method for vulcanizing rubber, wherein the oil-filled insoluble sulfur is used.
The invention has the beneficial effects that: the invention provides a preparation method of oil-filled insoluble sulfur, which comprises the steps of mixing a stabilizer with filling oil to obtain paste, and then mixing the paste with the insoluble sulfur to obtain the oil-filled insoluble sulfur. The oil-filled insoluble sulfur prepared by the method has good thermal stability, and the stability of the original oil-filled insoluble sulfur at 120 ℃ for 15min can be improved by more than 45 percent, so that the requirement of the high-stability insoluble sulfur meeting the production requirement of all-steel radial tires in the prior art is met and exceeded, the particle size of the insoluble sulfur is further integrated, the particle size distribution range of the insoluble sulfur is further concentrated, the dispersibility is improved, and the product use performance is optimized. The oil-filled insoluble sulfur provided by the invention is prepared by the method, has good thermal stability at 120 ℃ for 15min, reaches the standards of the same industry in foreign countries, and breaks through the monopoly of foreign countries.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow of a process for preparing oil-extended insoluble sulfur according to examples and comparative examples of the present invention;
FIG. 2 IS a graph showing a distribution of particle sizes of IS90 used as a raw material in a process for producing oil-extended insoluble sulfur according to example 20 of the present invention;
fig. 3 is a particle size distribution diagram of oil-extended insoluble sulfur prepared by the method for preparing oil-extended insoluble sulfur provided in example 20 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of oil-extended insoluble sulfur, which comprises the following raw materials: insoluble sulphur, extender oil and a stabilizer.
The common insoluble sulfur is powdery, is easy to fly and inconvenient to transport, and is difficult to be uniformly dispersed in rubber in the rubber processing and using process, so that certain pollution is caused to the environment. Therefore, the insoluble sulfur needs to be subjected to oil filling treatment to prevent dust generation and also to ensure that the insoluble sulfur and the oil are combined and then are more easily dispersed in the rubber. Insoluble sulfur belongs to an unstable structure, and if the insoluble sulfur is not subjected to stabilization treatment, a linear polymerization sulfur atom chain is broken at a higher speed from two ends and is finally converted into stable orthorhombic sulfur at normal temperature, so that a stabilizer is added during preparation of oil-filled insoluble sulfur, sulfur atoms at two ends of the sulfur atom chain reach a stable structure, the breaking speed of the sulfur atom chain is inhibited, the conversion to solubility is delayed, the thermal stability of the oil-filled insoluble sulfur is improved, and the oil-filled insoluble sulfur with better quality is obtained.
The stabilizer comprises one or more of DM, PR-75 and PR-85, and is preferably a composite stabilizer consisting of DM and PR-75 or a composite stabilizer consisting of DM and PR-85.
Wherein DM is dibenzothiazyl disulfide; PR-75 is a PR-75 type rubber dispersant; PR-85 is a PR-85 type rubber dispersant.
In an alternative embodiment, the amount of DM is 0.2 to 0.9% by mass of the insoluble sulfur, and may be, for example, but not limited to, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%, preferably 0.4% by mass of the insoluble sulfur; the amount of PR-75 is 0.3-0.8% by mass of insoluble sulfur, and may be, for example, but not limited to, 0.3%, 0.4%, 0.5%, 0.6%, 0.7% or 0.8%, preferably 0.6% by mass of insoluble sulfur; the amount of PR-85 is 0.3-0.8% by mass of insoluble sulfur, and may be, for example, but not limited to, 0.3%, 0.4%, 0.5%, 0.6%, 0.7% or 0.8%, and preferably 0.55% by mass of insoluble sulfur.
In an alternative embodiment, the mass fraction of insoluble sulfur in the insoluble sulfur is from 90% to 100%. The content of insoluble sulfur in the raw material is improved, so that the stability of the oil-extended insoluble sulfur can be further improved.
In an alternative embodiment, the filling oil may be, for example, but not limited to, naphthenic oil, aromatic oil, or white oil, and optionally, the filling oil may be one or more of naphthenic oil, aromatic oil, or white oil; naphthenic oils are preferred.
Optionally, the amount of the extender oil is 2% to 33% of the mass of the insoluble sulfur, and may be, for example, but not limited to, 2%, 8%, 12%, 15%, 17%, 22%, 27%, 32%, or 33%, and preferably 20% of the mass of the insoluble sulfur.
The preparation method of the oil-extended insoluble sulfur provided by the invention comprises the following steps: mixing stabilizer with filling oil to obtain paste, and mixing the paste with insoluble sulfur to obtain oil-extended insoluble sulfur. The method for producing oil-extended insoluble sulfur according to the present invention does not limit the mixing manner of the stabilizer and the extender oil, and may be carried out by mixing them uniformly, or the mixing manner of the paste and the insoluble sulfur may be also limited.
Optionally, in the present invention, the stabilizer is mixed with the extender oil using a tubing pump to obtain a paste; optionally, the paste in the pipeline pump is pumped into a mixer through a pump head, and is sprayed into the insoluble sulfur powder to be uniformly mixed.
In an alternative embodiment, the method of manufacture further comprises the step of comminuting the insoluble sulphur prior to mixing. Alternatively, the insoluble sulfur is pulverized to 50 to 150 mesh, for example, but not limited to, 50 mesh, 70 mesh, 90 mesh, 100 mesh, 130 mesh, 140 mesh or 150 mesh, preferably 100 mesh.
In an alternative embodiment, the mixing time of the paste and the insoluble sulfur is 10-30min, for example, but not limited to, 10min, 12min, 15min, 20min, 25min or 30min, preferably 15 min.
The invention provides oil-extended insoluble sulfur which is prepared by the preparation method.
In an alternative embodiment, the oil-extended insoluble sulfur has a thermal stability of 45% to 60% at 120 ℃.
The invention provides application of the oil-filled insoluble sulfur in rubber vulcanization.
The invention provides a method for vulcanizing rubber, which uses the oil-filled insoluble sulfur.
The oil-filled insoluble sulfur provided by the invention is applied to rubber vulcanization, has good thermal stability, and can optimize the product performance.
The advantageous effects of the present invention will be further described below with reference to examples and comparative examples.
The PR-75 type rubber dispersant used in the embodiment of the invention and the comparative example IS purchased from Qingdao Yinuo Xin chemical industry Co., Ltd, the PR-85 type rubber dispersant IS purchased from Qingdao Yinuo chemical industry Co., Ltd, and the insoluble sulfur IS90 used in the embodiment of the invention IS detected to have the average thermal stability of 30% at 120 ℃ for 15 min. Other practical and equipment used in the examples and comparative examples of the present invention are commercially available conventional instruments and equipment. The process flow of the preparation method of the oil-extended insoluble sulfur provided in the examples and comparative examples is shown in fig. 1.
Example 1-example 38
Examples 1 to 38 provide a method for producing oil-extended insoluble sulfur, and the raw materials and the amounts of the raw materials used in the method for producing oil-extended insoluble sulfur provided in examples 1 to 38 are shown in table 1, wherein the extended oil is naphthenic oil; filling oil (%) is the mass percentage of filling oil in insoluble sulfur; DM (%) is the mass percentage of DM in insoluble sulfur; PR-75 (%) is the mass percentage of PR-75 in insoluble sulfur; PR-85 (%) is the mass percentage of PR-85 in insoluble sulfur; IS90 IS insoluble sulfur with the mass fraction of insoluble sulfur being more than or equal to 90%; wherein the particle size distribution diagram of the raw material IS90 used in example 20 IS shown in FIG. 2, and the particle size distribution diagram of the oil-extended insoluble sulfur prepared by the method for preparing oil-extended insoluble sulfur provided in example 20 IS shown in FIG. 3.
Table 1 examples 1-38 provide the raw materials and amounts thereof for the preparation of oil-extended insoluble sulfur
Examples 1-38 provide a process for the preparation of oil-extended insoluble sulfur having the following process steps:
(a) mixing the stabilizing agent into naphthenic oil at normal temperature and mixing the stabilizing agent into the naphthenic oil by using a pipeline pump to obtain paste;
(b) pulverizing insoluble sulfur into powder;
(c) pumping the paste in the pipeline pump into a mixer through a pump head, spraying the paste into insoluble sulfur powder, and uniformly stirring to obtain the oil-filled insoluble sulfur product.
Wherein, the parameters of the process steps of the preparation method of the oil-filled insoluble sulfur are shown in table 2, wherein, the grinding mesh number represents the grinding mesh number of the insoluble sulfur in the step (b); the mixing time represents the mixing time for mixing the paste and the insoluble sulfur in the step (c).
Table 2 examples 1-examples 38 provide process parameters for the preparation of oil-extended insoluble sulfur
Comparative examples 1 to 19
Comparative examples 1 to 19 provide a method for preparing oil-extended insoluble sulfur, and raw materials and amounts thereof used in the method for preparing oil-extended insoluble sulfur provided in comparative examples 1 to 19 are shown in table 3, wherein the extended oil is naphthenic oil; filling oil (%) is the mass percentage of filling oil in insoluble sulfur; DM (%) is the mass percentage of DM in insoluble sulfur; PR-75 (%) is the mass percentage of PR-75 in insoluble sulfur; PR-85 (%) is the mass percentage of PR-85 in insoluble sulfur; IS90 IS insoluble sulfur with the mass fraction of insoluble sulfur being more than or equal to 90%.
Table 3 raw materials and amounts thereof used in the process for producing oil-extended insoluble sulfur provided in comparative examples 1 to 19
The process steps of the preparation method of the oil-extended insoluble sulfur provided in comparative examples 1 to 16 are as follows:
(a) mixing the stabilizing agent into naphthenic oil at normal temperature and mixing the stabilizing agent into the naphthenic oil by using a pipeline pump to obtain paste;
(b) pulverizing insoluble sulfur into powder;
(c) pumping the paste in the pipeline pump into a mixer through a pump head, spraying the paste into insoluble sulfur powder, and uniformly stirring to obtain the oil-filled insoluble sulfur product.
Wherein, the parameters of the process steps of the preparation method of the oil-filled insoluble sulfur are shown in table 2, wherein, the grinding mesh number represents the grinding mesh number of the insoluble sulfur in the step (b); the mixing time represents the mixing time for mixing the paste and the insoluble sulfur in the step (c).
Table 4 process parameters of the preparation method of oil-extended insoluble sulfur provided in comparative example 1 to comparative example 16
| Grinding mesh number (mesh) | Mixing time (min) | |
| Comparative examples 1 to 11 | 100 | 15 |
| Comparative examples 12 and 16 | 20 | 15 |
| Comparative example 13 | 200 | 15 |
| Comparative example 14 | 100 | 5 |
| Comparative example 15 | 100 | 40 |
Examples of effects
The properties of the oil-extended insoluble sulfur prepared by the preparation method of the oil-extended insoluble sulfur provided in the above examples and comparative examples were measured according to the method provided in the chemical industry standard HG/T2525-2011 of the people's republic of china, and the results are shown in table 5:
TABLE 5 Properties of oil-extended insoluble Sulfur
As can be seen from the data in the table, the oil-extended insoluble sulfur prepared by the preparation method of the oil-extended insoluble sulfur provided in examples 1-38 has higher thermal stability at 120 ℃ for 15 min.
Among them, it can be seen from the comparison of example 1 to example 15 with example 20 to example 25 that the use of a composite stabilizer is superior to the use of a single stabilizer; it can be seen from comparison of examples 1-25 with comparative examples 1-9 that the thermal stability of oil-extended insoluble sulfur can be improved by the use of suitable stabilizers, wherein examples 20 and 25 provide the same stabilizers and the dosages used therefor as the other examples; and it can be seen from example 26 that example 20 and example 25 are more preferable in view of production cost, since the formulation of the composite stabilizer provided in examples 20 and 25 is not due to the use of DM, PR-75 and PR-85 as the composite stabilizer.
In the present embodiment, the naphthenic oil is used in an amount that affects the thermal stability of the oil-extended insoluble sulfur, as shown by comparing examples 27 to 30 with comparative examples 10 to 11, and the naphthenic oil filling 20% of the insoluble sulfur can provide higher thermal stability of the oil-extended insoluble sulfur.
As can be seen from the comparison between example 31-practical example 38 and comparative example 12-comparative example 16, the process parameters of the preparation method of the oil-extended insoluble sulfur provided by the invention are optimized, so that the thermal stability of the prepared oil-extended insoluble sulfur at 120 ℃ for 15min is obviously improved.
As can be seen from a comparison between fig. 2 and fig. 3, the method for preparing oil-extended insoluble sulfur provided in example 20 further integrates the particle size of the insoluble sulfur, so that the particle size distribution range of the insoluble sulfur is further concentrated, the dispersibility is improved, and the usability of the product is optimized.
In conclusion, the preparation method of the oil-extended insoluble sulfur provided by the invention has the advantage that the thermal stability of the prepared oil-extended insoluble sulfur is obviously improved at 120 ℃ for 15min by optimizing raw materials and processes.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (14)
1. The preparation method of the oil-extended insoluble sulfur is characterized by comprising the following steps: mixing the stabilizer with filling oil to obtain paste, and mixing the paste with insoluble sulfur to obtain oil-filled insoluble sulfur;
the stabilizer is a composite stabilizer consisting of dibenzothiazyl disulfide and a PR-75 type rubber dispersant or a composite stabilizer consisting of dibenzothiazyl disulfide and a PR-85 type rubber dispersant;
the dosage of the dibenzothiazyl disulfide is 0.2-0.9% of the mass of the insoluble sulfur, the dosage of the PR-75 type rubber dispersant is 0.3-0.8% of the mass of the insoluble sulfur, and the dosage of the PR-85 type rubber dispersant is 0.3-0.8% of the mass of the insoluble sulfur.
2. The preparation method of claim 1, wherein the dibenzothiazyl disulfide is used in an amount of 0.3-0.6% by mass of the insoluble sulfur, the PR-75 type rubber dispersant is used in an amount of 0.5-0.7% by mass of the insoluble sulfur, and the PR-85 type rubber dispersant is used in an amount of 0.5-0.7% by mass of the insoluble sulfur.
3. The preparation method according to claim 2, wherein the dibenzothiazyl disulfide is used in an amount of 0.4% by mass of insoluble sulfur, the PR-75 type rubber dispersant is used in an amount of 0.6% by mass of insoluble sulfur, and the PR-85 type rubber dispersant is used in an amount of 0.55% by mass of insoluble sulfur.
4. The preparation method according to claim 1, wherein the mass fraction of insoluble sulfur in the insoluble sulfur is 90% to 100%.
5. The process according to claim 1, wherein the extender oil is used in an amount of 2% to 33% by mass of insoluble sulphur.
6. The preparation method according to claim 5, wherein the extender oil is used in an amount of 10-30% by mass of the insoluble sulfur.
7. The process according to claim 6, wherein the extender oil is used in an amount of 20% by mass of insoluble sulphur.
8. The process of claim 1, further comprising the step of comminuting the insoluble sulfur prior to mixing.
9. The method according to claim 8, wherein the insoluble sulfur is pulverized to 50 to 150 mesh.
10. The process according to claim 1, wherein the paste is mixed with the insoluble sulphur for a period of time ranging from 10 to 30 min.
11. An oil-extended insoluble sulfur, which is produced by the production method according to any one of claims 1 to 10.
12. The oil-extended insoluble sulfur of claim 11, wherein the oil-extended insoluble sulfur has a thermal stability of 45 to 60% at 120 ℃.
13. Use of the oil-extended insoluble sulfur of claim 11 or 12 for rubber vulcanization.
14. A method for vulcanizing rubber, characterized in that the oil-extended insoluble sulfur according to claim 11 or 12 is used in the method.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240192A (en) * | 1999-04-26 | 2000-01-05 | 赵水斌 | Process for preparing insoluble sulphur and productive equipment |
| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| 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 |
| 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 |
-
2017
- 2017-12-22 CN CN201711415263.9A patent/CN108129693B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240192A (en) * | 1999-04-26 | 2000-01-05 | 赵水斌 | Process for preparing insoluble sulphur and productive equipment |
| 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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