CN115417383B - Application of polyethylene glycol fatty acid ester in improving dispersibility of insoluble sulfur - Google Patents
Application of polyethylene glycol fatty acid ester in improving dispersibility of insoluble sulfur Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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Abstract
The invention provides application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur, and belongs to the technical field of sulfur preparation. According to the invention, polyethylene glycol fatty acid ester is added into insoluble sulfur, so that the dispersibility of the insoluble sulfur can be improved, and the product quality can be ensured.
Description
Technical Field
The invention belongs to the technical field of sulfur preparation, and particularly relates to application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur.
Background
The insoluble sulfur is also called elastic sulfur or polymeric sulfur, is a linear polymer formed by polymerizing a large number of sulfur atoms, has a relative molecular mass of tens of thousands, is nontoxic and combustible yellow powder, is named as insoluble carbon disulfide, and is an allotrope and polymer modified variety of common sulfur in a high polymerization form.
The insoluble sulfur is used as an important vulcanizing agent in the rubber industry, has excellent vulcanizing property, can improve the adhesive strength of rubber materials and framework materials, effectively prevents the rubber materials from being frosted, and improves the heat resistance and wear resistance of the tire. Therefore, the rubber composition is widely applied to tire components and rubber products, such as tire carcasses, buffer layers, sidewalls, rubber tubes, rubber belts and the like, which are required to have high adhesive strength with framework materials, and can also be applied to cables, rubber editions, rubber shoes, oil seals and rubber compositions of other light-color rubber products with large sulfur consumption. The dispersion performance of the insoluble sulfur plays a vital role in the application of the product, and the dispersion performance of the insoluble sulfur directly affects the mixing uniformity of the sulfur and the sizing material, so that the dispersion performance of the insoluble sulfur has a larger influence on the service performance and the service life of the rubber product.
In the prior art, an antistatic agent is usually added in the production process of insoluble sulfur to improve the dispersibility of the insoluble sulfur, but the addition of the antistatic agent usually causes the performance and quality of a product to be reduced to a certain extent, and particularly has a great influence on the thermal stability of the product. At present, fatty alcohol polyoxyethylene ether is used as an antistatic agent to be added into insoluble sulfur, so that the dispersibility of the insoluble sulfur can be improved to a certain extent, but the fatty alcohol polyoxyethylene ether is explosive and is inconvenient to prepare, transport and use. Therefore, on the basis of effectively improving the antistatic performance and the dispersing performance of the obtained insoluble sulfur product, the method for preventing the serious decline of other performances and quality of the product has important significance, and is also a key difficulty in the sulfur production process.
Disclosure of Invention
The invention provides application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur, and the polyethylene glycol fatty acid ester is added into the insoluble sulfur, so that the dispersibility of the insoluble sulfur can be improved, and the product quality can be ensured.
In order to achieve the above purpose, the invention provides an application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur.
Preferably, the polyethylene glycol fatty acid ester comprises a polyethylene glycol chain and an alkyl chain; the ratio of the polyethylene glycol chain segment to the alkyl chain segment is 1:1 to 2.
Preferably, the molecular weight of the polyethylene glycol chain is 200-2000; the molecular weight of the alkyl chain is 80-800.
Preferably, the addition amount of the polyethylene glycol fatty acid ester is 0.3-0.5% of the mass of the insoluble sulfur.
Preferably, the insoluble sulfur is prepared by the following steps:
1) Preparing insoluble sulfur crude product by adopting a low temperature-melting method to sulfur powder;
2) Extracting, drying, sieving and oil-filling the insoluble sulfur crude product in sequence to obtain insoluble sulfur; wherein polyethylene glycol fatty acid ester is added in the oil-filling treatment process.
Preferably, the preparation of the insoluble sulfur crude product by the low-temperature-melting method in the step 1) comprises the following steps:
a. melting the sulfur powder at 120-150 ℃ to obtain liquid sulfur;
b. adding a stabilizer into the liquid sulfur, heating to 200-250 ℃, preserving heat for 0.5-20 h, and then quenching in an aqueous medium to obtain a viscoelastic polymer;
c. and tabletting, drying and crushing the viscoelastic polymer in sequence to obtain an insoluble sulfur crude product.
Preferably, the stabilizer is one or more of halogen stabilizers, olefin stabilizers and redox system stabilizers; the addition amount of the stabilizer is 0.1-0.2% of the mass of the liquid sulfur.
Preferably, the drying temperature in the step c is 55-60 ℃ and the time is 4-6 h.
Preferably, the oil-filling treatment in the step 2) is performed in the following manner: mixing the insoluble sulfur after sieving with naphthenic oil; the mass ratio of the insoluble sulfur to the naphthenic oil after sieving is (79-81): (19-21).
Preferably, in the step 2), carbon disulfide is used for extraction.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the invention, polyethylene glycol fatty acid ester is added into insoluble sulfur, so that on one hand, the polyethylene glycol chain segment of the substance can effectively lead out static electricity; on the other hand, the substance also contains alkyl chains, can be well fused with rubber oil, and further improves the dispersibility of insoluble sulfur; in addition, the antistatic and dispersing properties of the material can be adjusted by adjusting the ratio of the polyethylene glycol segment to the alkyl segment. Therefore, the insoluble sulfur using the antistatic agent has good dispersibility, thereby improving the quality of the prepared rubber. Meanwhile, the method provided by the invention is simple to operate and mild in condition.
Drawings
FIG. 1 is a graph showing the thermal stability of sulfur prepared in example 2;
FIG. 2 is a graph showing the thermal stability of sulfur prepared in comparative example 2.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides an application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur.
In the present invention, the polyethylene glycol fatty acid ester preferably includes a polyethylene glycol chain and a fatty acid chain; the ratio of polyethylene glycol segment to alkyl segment is preferably 1:1 to 2.
In the present invention, the molecular weight of the polyethylene glycol chain is preferably 200 to 2000, more preferably 400 to 1000; the molecular weight of the fatty acid chain is preferably 80 to 800, more preferably 200 to 600.
In the present invention, the amount of the polyethylene glycol fatty acid ester added is preferably 0.3 to 0.5% by mass of the insoluble sulfur.
In the invention, the polyethylene glycol fatty acid ester is added in the oil-filling process of insoluble sulfur. According to the invention, polyethylene glycol fatty acid ester is added into insoluble sulfur, so that on one hand, the polyethylene glycol chain segment of the substance can effectively lead out static electricity; on the other hand, the substance also contains a fatty chain, can be well fused with rubber oil, and further improves the dispersibility of insoluble sulfur; in addition, the antistatic and dispersing properties of the material can be adjusted by adjusting the ratio of the polyethylene glycol segment to the alkyl segment. Meanwhile, better thermal stability can be ensured.
In the invention, the insoluble sulfur is preferably prepared by the following steps:
1) Preparing insoluble sulfur crude product by adopting a low temperature-melting method to sulfur powder;
2) Extracting, drying, sieving and oil-filling the insoluble sulfur crude product in sequence to obtain insoluble sulfur; wherein polyethylene glycol fatty acid ester is added in the oil-filling treatment process.
The invention prepares the insoluble sulfur crude product by adopting a low temperature-melting method to sulfur powder. In the invention, the preparation of the insoluble sulfur crude product by the low-temperature melting method preferably comprises the following steps:
a. melting the sulfur powder at 120-150 ℃ to obtain liquid sulfur;
b. adding a stabilizer into the liquid sulfur, heating to 200-250 ℃, preserving heat for 0.5-20 h, and then quenching in an aqueous medium to obtain a viscoelastic polymer;
c. and tabletting, drying and crushing the viscoelastic polymer in sequence to obtain an insoluble sulfur crude product.
In the invention, the stabilizer is preferably one or more of halogen stabilizers, olefin stabilizers and redox system stabilizers; the halogen stabilizer preferably comprises ferric chloride, phosphorus trichloride, phosphorus pentachloride, carbon tetrachloride, silicon tetrachloride, sulfur dichloride, sulfur oxychloride, phosphorus oxychloride or titanium tetrachloride; the olefinic stabilizer preferably comprises dodecene, tetradecene, octadecene, benzocyclopropene, chloroprene, isoprene, turpentine, terpineol, terpene; the addition amount of the stabilizer is preferably 0.1-0.2% of the mass of the liquid sulfur. In the invention, after the sulfur atoms of the stabilizer are added to polymerize into insoluble sulfur, both ends of a polymerized long chain are still in a free radical state, and the electrons of the outer layers of the sulfur atoms at both ends can reach 8 to form a stable structure by adding the stabilizer, so that the chain breakage of the polymerized sulfur atoms is inhibited and the sulfur atoms are converted into soluble sulfur. In the present invention, the particle size of the pulverization is preferably 10 to 150. Mu.m. In the present invention, the holding time is preferably 0.5 to 20 hours, more preferably 2 to 4 hours.
In the present invention, the temperature of the drying in the step c is preferably 55 to 60 ℃ and the time is preferably 4 to 6 hours.
After obtaining an insoluble sulfur crude product, sequentially extracting, drying, sieving and oil-filling the insoluble sulfur crude product to obtain insoluble sulfur; wherein polyethylene glycol fatty acid ester is added in the oil-filling treatment process. In the present invention, the extraction is preferably performed with carbon disulphide. In the present invention, the drying temperature is preferably 55 to 60℃and the drying time is preferably 2 to 3 hours. In the present invention, the pore diameter of the sieve used in the sieving is preferably 100 mesh. In the present invention, the oil-filling treatment is preferably performed by: mixing the insoluble sulfur after sieving with naphthenic oil; the mass ratio of the insoluble sulfur to the naphthenic oil after sieving is preferably (79-81): (19-21).
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Melting the sulfur powder at 120 ℃ to obtain liquid sulfur. Adding stabilizer ferric trichloride (the addition amount of the stabilizer is 0.1% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 230 ℃, preserving heat for 1.2h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 55deg.C for 6 hr, and pulverizing (particle size of 10-120 μm) to obtain insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 55deg.C for 2 hr, sieving with 100 mesh sieve, and collecting sieved undersize, naphthenic oil and polyethylene glycol fatty acidThe ester (polyethylene glycol fatty acid ester has a molecular weight of 751, polyethylene glycol chain has a molecular weight of 400, fatty acid has a molecular weight of 369, and a ratio of polyethylene glycol chain segment to fatty acid chain segment is 1:1) is mixed according to a mass ratio of 79:21:0.237, and oil-filled, and after oil-filled, the mixture is sieved by a 100-mesh sieve again to obtain insoluble sulfur.
Example 2
Melting the sulfur powder at 140 ℃ to obtain liquid sulfur. Adding phosphorus oxychloride as a stabilizer (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 200 ℃, preserving heat for 1h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in a baking oven at 55 ℃ for 6 hours, and crushing (the granularity after crushing is 5-150 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 55deg.C for 2 hr, sieving with 100 mesh sieve, mixing the sieved undersize, naphthenic oil and polyethylene glycol fatty acid ester (molecular weight of polyethylene glycol fatty acid ester is 800, molecular weight of polyethylene glycol chain is about 400, molecular weight of fatty acid is about 200, and ratio of polyethylene glycol chain segment to fatty acid chain segment is 1:2) according to mass ratio of 80:20:0.32, and sieving with 100 mesh sieve again to obtain insoluble sulfur. The thermal stability of the insoluble sulfur prepared is shown in figure 1.
Example 3
Melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 250 ℃, preserving heat for 0.8h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 60deg.C for 2 hr, sieving with 100 mesh sieve, sievingThe material, naphthenic oil and polyethylene glycol fatty acid ester (the molecular weight of the polyethylene glycol fatty acid ester is 771, the molecular weight of the polyethylene glycol chain is about 200, the molecular weight of the fatty acid chain is about 285.45, the ratio of the polyethylene glycol chain segment to the fatty acid chain segment is 1:2) are mixed according to the mass ratio of 81:19:0.405, oil filling treatment is carried out, and after oil filling is finished, the mixture is sieved by a 100-mesh sieve again, so as to obtain insoluble sulfur.
Example 4
Melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 200 ℃, preserving heat for 20 hours, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 60 ℃ for 2h, sieving with a 100-mesh sieve, mixing the sieved undersize, naphthenic oil and polyethylene glycol fatty acid ester (the molecular weight of the polyethylene glycol fatty acid ester is 2313, the molecular weight of the polyethylene glycol chain is 1800, the molecular weight of the fatty acid chain is 256.4, and the ratio of the polyethylene glycol chain segment to the fatty acid chain segment is 1:2) according to the mass ratio of 81:19:0.405, filling oil, and sieving with the 100-mesh sieve again after filling oil, thus obtaining insoluble sulfur.
Example 5
Melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 250 ℃, preserving heat for 0.8h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 60deg.C for 2 hr, sieving with 100 mesh sieve, collecting sieved undersize,The naphthenic oil and polyethylene glycol fatty acid ester (the molecular weight of the polyethylene glycol fatty acid ester is 1200, the molecular weight of the polyethylene glycol chain is about 1000, the molecular weight of the fatty acid chain is about 200, the ratio of the polyethylene glycol chain segment to the fatty acid chain segment is 1:1) are mixed according to the mass ratio of 81:19:0.405, oil filling treatment is carried out, and after oil filling is finished, the mixture is sieved by a 100-mesh sieve again, so as to obtain insoluble sulfur.
Comparative example 1
The difference from example 3 is that no polyethylene glycol fatty acid ester is added during the oil-filling process, and the specific operation is as follows:
melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 250 ℃, preserving heat for 0.8h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 60 ℃ for 2 hours, sieving with a 100-mesh sieve, mixing the sieved undersize and naphthenic oil according to the mass ratio of 81:19, carrying out oil filling treatment, and sieving with the 100-mesh sieve again after oil filling is finished to obtain insoluble sulfur.
Comparative example 2
The difference from example 3 is that polyethylene glycol is added as a dispersant in the oil-filling process, and the specific operation is as follows:
melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 250 ℃, preserving heat for 0.8h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, and then atAnd (3) drying at 60 ℃ for 2 hours, sieving with a 100-mesh sieve, mixing the sieved undersize, naphthenic oil and polyethylene glycol (the molecular weight of the polyethylene glycol is about 600) according to the mass ratio of 81:19:0.405, carrying out oil filling treatment, and sieving with the 100-mesh sieve again after the oil filling is finished to obtain insoluble sulfur. The thermal stability of the insoluble sulfur prepared is shown in figure 2.
As can be seen from a comparison of fig. 1 and 2, the sulfur prepared in example 2 has a thermal phase transition starting point of 114.6 ℃ which is much higher than 102.5 ℃ of comparative example 1. The peak heated phase transition of sulfur prepared in example 2 was 123.6 ℃ which is much higher than 107.4 ℃ of comparative example 2. The above demonstrates that the thermal stability of example 2 is better than that of comparative example 2.
Comparative example 3
The difference from example 2 is that polyethylene glycol and fatty acid are added during the oil-filling process, respectively, the specific operations are as follows:
melting the sulfur powder at 150 ℃ to obtain liquid sulfur. Adding stabilizer terpene (the addition amount of the stabilizer is 0.2% of the mass of the liquid sulfur) into the obtained liquid sulfur, heating to 250 ℃, preserving heat for 0.8h, and then quenching in an aqueous medium to obtain a viscoelastic polymer; tabletting the viscoelastic polymer, drying in an oven at 60 ℃ for 4 hours, and crushing (the granularity after crushing is 15-110 mu m) to obtain an insoluble sulfur crude product.
The obtained insoluble sulfur crude product adopts CS 2 Extracting, drying at 60 ℃ for 2 hours, sieving with a 100-mesh sieve, mixing sieved undersize, naphthenic oil, polyethylene glycol (the molecular weight of the polyethylene glycol is about 600) and palmitic acid according to the mass ratio of 81:19:2:1, carrying out oil filling treatment, and sieving with the 100-mesh sieve again after oil filling is finished to obtain insoluble sulfur.
Performance testing
The antistatic effect of insoluble vulcanization prepared in the above examples and comparative examples was tested, and the specific results are shown in table 1.
TABLE 1 antistatic Effect
The insoluble vulcanizates prepared in the above examples and comparative examples were tested for thermal stability and the specific results are shown in table 2.
TABLE 2 thermal stability
As can be seen from tables 1 and 2, the electrostatic values of examples 1 to 5 and comparative examples 2 to 3 are lower than that of comparative example 1, indicating that examples 1 to 5 and comparative examples 2 to 3 are effective in improving the dispersibility of the obtained products, but that comparative examples 2 to 3 are inferior in dispersibility to example 3 and that comparative examples 2 and 3 are inferior in thermal stability.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The application of polyethylene glycol fatty acid ester in improving the dispersibility of insoluble sulfur;
the polyethylene glycol fatty acid ester comprises a polyethylene glycol chain and an alkyl chain; the ratio of polyethylene glycol segment to alkyl segment is 1: 1-2;
the molecular weight of the polyethylene glycol chain is 200-2000; the molecular weight of the alkyl chain is 80-800;
the addition amount of the polyethylene glycol fatty acid ester is 0.3-0.5% of the mass of insoluble sulfur;
the insoluble sulfur is prepared by the following steps:
1) Preparing insoluble sulfur crude product by adopting a low temperature-melting method to sulfur powder;
2) Extracting, drying, sieving and oil-filling the insoluble sulfur crude product in sequence to obtain insoluble sulfur; wherein polyethylene glycol fatty acid ester is added in the oil-filling treatment process.
2. The use according to claim 1, wherein the low temperature-melting process of step 1) for preparing crude insoluble sulphur comprises the steps of:
a. melting the sulfur powder at 120-150 ℃ to obtain liquid sulfur;
b. adding a stabilizer into the liquid sulfur, heating to 200-250 ℃, preserving heat for 0.5-20 h, and then quenching in an aqueous medium to obtain a viscoelastic polymer;
c. and tabletting, drying and crushing the viscoelastic polymer in sequence to obtain an insoluble sulfur crude product.
3. The use according to claim 2, wherein the stabilizer is one or more of halogen-based stabilizers, olefin-based stabilizers and redox system stabilizers; the addition amount of the stabilizer is 0.1-0.2% of the mass of the liquid sulfur.
4. The use according to claim 2, wherein the drying in step c is carried out at a temperature of 55-60 ℃ for a time of 4-6 hours.
5. The use according to claim 1, wherein the oil-filled treatment in step 2) is performed by: mixing the insoluble sulfur after sieving with naphthenic oil; the mass ratio of the insoluble sulfur to the naphthenic oil after sieving is (79-81): (19-21).
6. The use according to claim 1, wherein in step 2) carbon disulphide is used for the extraction.
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