CN105540552A - Preparation method of pressure-resisting sulphur with high bonding strength - Google Patents
Preparation method of pressure-resisting sulphur with high bonding strength Download PDFInfo
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- CN105540552A CN105540552A CN201610048694.5A CN201610048694A CN105540552A CN 105540552 A CN105540552 A CN 105540552A CN 201610048694 A CN201610048694 A CN 201610048694A CN 105540552 A CN105540552 A CN 105540552A
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- sulphur
- powder
- sio
- denaturing agent
- sex change
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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
- C01B17/0243—Other after-treatment of sulfur
- C01B17/0248—Other after-treatment of sulfur of particulate sulfur
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of pressure-resisting sulphur with high bonding strength. The method comprises the steps that a sulphur raw material is heated to reach 130-160 DEG C to be a melt, a sulphur denaturing agent at the temperature of 50-70 DEG C is slowly added, slight stirring is carried out for 10-20 min, the temperature is increased to 140-170 DEG C then kept for 0.5-2 h to obtain a denatured sulphur melt, silicon dioxide powder is sieved by a sieve with 60-120 meshes after being smashed and placed into a vacuum drying oven in advance to be dried for 12-24 h, and the dried silicon dioxide powder is heated to reach 130-180 DEG C to be mixed with the denatured sulphur melt at the temperature of 140-170 DEG C for solidification. The internal structure interconnection of sulphur is stronger by adding the sulphur denaturing agent, the bonding strength of the sulphur is effectively increased, the internal stress problem produced by macroscopic volume changes caused by phase transformation of the sulphur in the cooling process is effectively solved due to the dispersion strengthening effect and pinning effect inside the sulphur material, and the cooled and solidified sulphur material is better in pressure resistance strength.
Description
Technical field
The present invention relates to sulphur preparing technical field, be specifically related to a kind of resistance to compression, sulphur preparation method that cohesive strength is high.
Background technology
Sulphur as subsidiary material common in a kind of material of construction, widespread use and offshore structure, bearing etc. when highway, bridge, airfield runway and hardstand, water shoot and Jiao Jing, railroad sleeper mechanism, bridge zero.But, sulphur becomes viscosity small flow good fluid when being warming up to 130-160 DEG C, restore during cooling and become solid, can amorphous sulfur be generated when speed is cold, in process of cooling, macroscopical volume-diminished can be caused because the chemical structure of sulphur inside changes, inner generation string stress, and then cause the internal structure of sulphur to be destroyed, its physical strength is as ultimate compression strength, and the degradations such as cohesive strength, lose use value.In order to improve physical strength and the toughness of sulphur, stop the defective expansion in matrix Central Plains and continue the appearance in new crack, generally can mix a small amount of properties-correcting agent in sulphur and its congruent melting mixes in the past, effectively can solve the problem because internal stress causes physical strength to reduce when cooled, the sulphur of modification has good cohesive strength and ultimate compression strength at normal temperatures.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of resistance to compression, sulphur preparation method that cohesive strength is high, improve ultimate compression strength and the cohesive strength of sulphur with this, for achieving the above object, the present invention is achieved through the following technical solutions:
Element sulfur raw material is heated to 130-160 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 50-70 DEG C, stir 10-20 minute gently, be incubated 0.5-2 hour after being warming up to 140-170 DEG C and obtain sex change sulfur melting thing, cross 60-120 mesh sieve after being pulverized by SiO 2 powder and be put into dry 12-24 hour in vacuum drying oven in advance, dried SiO 2 powder is heated to 130 DEG C-180 DEG C to mix with described 140-170 DEG C of sex change sulfur melting thing, be circulated in container after mixing and be cooled to room temperature, be cured again, described element sulfur raw material and sulphur denaturing agent mass ratio are 1:4-1:6, described SiO 2 powder and sex change sulphur mass ratio are 1:3-1:5.
Preferably, described sulphur denaturing agent is the mixture of dicyclopentadiene and Vinyl toluene, and the mass ratio of dicyclopentadiene and Vinyl toluene is 4:1.
Preferably, the mass ratio of described sulphur denaturing agent and element sulfur raw material is 1:4.5.
Preferably, described SiO 2 powder crosses 120 mesh sieves after pulverizing.
Preferably, described SiO 2 powder puts into vacuum drying oven dry 20 hours in advance.
Preferably, the mass ratio of described SiO 2 powder and sex change sulfur melting thing is 1:4.
Preferably, described SiO 2 powder is heated to 140 DEG C and mixes with described sex change sulfur melting thing.
The invention provides a kind of resistance to compression, sulphur preparation method that cohesive strength is high, its beneficial effect is:
Element sulfur raw material mobility 160 DEG C time is better, better with the Combination of the sulphur denaturing agent added and SiO 2 powder, adding of denaturing agent makes the structure interconnectivity of sulphur inside stronger, thus the effective cohesive strength increasing sulphur, and by the dispersion-strengthened action of SiO 2 powder in sulfur material inside and pinning effect, effectively solve the internal stress problem that sulphur produces because phase transformation transformation causes macroscopical volume change in process of cooling, the sulfur material ultimate compression strength obtained after making cooling curing is better.In addition, the method for the invention can be easy and comparatively easily obtain described high resistance to compression, cohesive strength sulfur material.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with embodiments of the invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
Element sulfur raw material is heated to 130 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 60 DEG C, stir 15 minutes gently, after being warming up to 140 DEG C, insulation obtains sex change sulfur melting thing for 0.5 hour, cross 120 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 20 hours in advance, dried SiO 2 powder is heated to 140 DEG C to mix with described 140 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein sulphur denaturing agent and element sulfur raw material mass ratio are 1:4.5, wherein SiO 2 powder and sex change sulfur melting amount are than being 1:4.
Embodiment 2:
Element sulfur raw material is heated to 130 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 50 DEG C, stir 10 minutes gently, after being warming up to 140 DEG C, insulation obtains sex change sulfur melting thing for 0.5 hour, cross 60 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 12 hours in advance, dried SiO 2 powder is heated to 130 DEG C to mix with described 140 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein element sulfur raw material and sulphur denaturing agent mass ratio are 1:4, wherein SiO 2 powder and sex change sulphur mass ratio are 1:3.
Embodiment 3:
Element sulfur raw material is heated to 160 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 70 DEG C, stir 20 minutes gently, after being warming up to 170 DEG C, insulation obtains sex change sulfur melting thing for 2 hours, cross 120 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 24 hours in advance, dried SiO 2 powder is heated to 180 DEG C to mix with described 170 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein element sulfur raw material and sulphur denaturing agent mass ratio are 1:6, wherein SiO 2 powder and sex change sulphur mass ratio are 1:5.
Embodiment 4:
Element sulfur raw material is heated to 145 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 60 DEG C, stir 15 minutes gently, after being warming up to 155 DEG C, insulation obtains sex change sulfur melting thing for 1.5 hours, cross 120 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 18 hours in advance, dried SiO 2 powder is heated to 155 DEG C to mix with described 155 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein element sulfur raw material and sulphur denaturing agent mass ratio are 1:5, wherein SiO 2 powder and sex change sulphur mass ratio are 1:4.
Embodiment 5:
Element sulfur raw material is heated to 150 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 65 DEG C, stir 17 minutes gently, after being warming up to 152 DEG C, insulation obtains sex change sulfur melting thing for 1 hour, cross 120 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 13 hours in advance, dried SiO 2 powder is heated to 145 DEG C to mix with described 152 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein element sulfur raw material and sulphur denaturing agent mass ratio are 1:5.5, wherein SiO 2 powder and sex change sulphur mass ratio are 1:4.5.
Embodiment 6:
Element sulfur raw material is heated to 135 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 50 DEG C, stir 12 minutes gently, after being warming up to 155 DEG C, insulation obtains sex change sulfur melting thing for 2 hours, cross 60 mesh sieves after being pulverized by SiO 2 powder and to be put in vacuum drying oven dry 14 hours in advance, dried SiO 2 powder is heated to 160 DEG C to mix with described 155 DEG C of sex change sulfur melting things, be circulated in container after mixing and be cooled to room temperature, be cured again, wherein element sulfur raw material and sulphur denaturing agent mass ratio are 1:4.5, wherein SiO 2 powder and sex change sulphur mass ratio are 1:3.5.
Above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (7)
1. a resistance to compression, the sulphur preparation method that cohesive strength is high, it is characterized in that: element sulfur raw material is heated to 130-160 DEG C and becomes melts, slowly add the sulphur denaturing agent that temperature is 50-70 DEG C, stir 10-20 minute gently, be incubated 0.5-2 hour after being warming up to 140-170 DEG C and obtain sex change sulfur melting thing, cross 60-120 mesh sieve after being pulverized by SiO 2 powder and be put into dry 12-24 hour in vacuum drying oven in advance, dried SiO 2 powder is heated to 130 DEG C-180 DEG C to mix with described 140-170 DEG C of sex change sulfur melting thing, be circulated in container after mixing and be cooled to room temperature, be cured again, described element sulfur raw material and sulphur denaturing agent mass ratio are 1:4-1:6, described SiO 2 powder and sex change sulphur mass ratio are 1:3-1:5.
2. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: described sulphur denaturing agent is the mixture of dicyclopentadiene and Vinyl toluene, and the mass ratio of dicyclopentadiene and Vinyl toluene is 4:1.
3. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: the mass ratio of described sulphur denaturing agent and element sulfur raw material is 1:4.5.
4. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: described SiO 2 powder crosses 120 mesh sieves after pulverizing.
5. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: described SiO 2 powder puts into vacuum drying oven dry 20 hours in advance.
6. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: the mass ratio of described SiO 2 powder and sex change sulfur melting thing is 1:4.
7. resistance to compression according to claim 1, the sulphur preparation method that cohesive strength is high, is characterized in that: described SiO 2 powder is heated to 140 DEG C and mixes with described sex change sulfur melting thing.
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Citations (9)
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|---|---|---|---|---|
| US3647398A (en) * | 1969-03-21 | 1972-03-07 | Corp De Fomento De La Producti | Process for removing gangue from sulfur-bearing materials |
| CN1849273A (en) * | 2003-09-11 | 2006-10-18 | 新日本石油株式会社 | Sulfur intermediate material, sulfur material and process for producing the same |
| US20100084315A1 (en) * | 2006-10-05 | 2010-04-08 | Carolus Matthias Anna Maria Mesters | Process for treating elemental sulphur for smell improvement |
| CN102757214A (en) * | 2011-04-29 | 2012-10-31 | 青岛鼎基环境防护科技有限公司 | Sulfur-modified composite material used as corrosion-proof coating |
| CN102755957A (en) * | 2011-04-29 | 2012-10-31 | 刘岩 | Atomizing and spraying method of sulfur modified composite anticorrosive coating |
| CN102976282A (en) * | 2012-11-14 | 2013-03-20 | 江南大学 | Insoluble sulfur efficient stabilizer and preparation method thereof |
| CN103204479A (en) * | 2013-03-22 | 2013-07-17 | 上海京海（安徽）化工有限公司 | Production method for high-content insoluble sulfur |
| CN103318848A (en) * | 2013-05-23 | 2013-09-25 | 上海京海（安徽）化工有限公司 | Production method of high-dispersion high-thermal-stability insoluble sulfur |
| CN104692337A (en) * | 2015-02-11 | 2015-06-10 | 上海京海（安徽）化工有限公司 | Insoluble sulfur capable of improving wear resistance of rubber products and preparation method thereof |
-
2016
- 2016-01-22 CN CN201610048694.5A patent/CN105540552A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3647398A (en) * | 1969-03-21 | 1972-03-07 | Corp De Fomento De La Producti | Process for removing gangue from sulfur-bearing materials |
| CN1849273A (en) * | 2003-09-11 | 2006-10-18 | 新日本石油株式会社 | Sulfur intermediate material, sulfur material and process for producing the same |
| US20100084315A1 (en) * | 2006-10-05 | 2010-04-08 | Carolus Matthias Anna Maria Mesters | Process for treating elemental sulphur for smell improvement |
| CN102757214A (en) * | 2011-04-29 | 2012-10-31 | 青岛鼎基环境防护科技有限公司 | Sulfur-modified composite material used as corrosion-proof coating |
| CN102755957A (en) * | 2011-04-29 | 2012-10-31 | 刘岩 | Atomizing and spraying method of sulfur modified composite anticorrosive coating |
| CN102976282A (en) * | 2012-11-14 | 2013-03-20 | 江南大学 | Insoluble sulfur efficient stabilizer and preparation method thereof |
| CN103204479A (en) * | 2013-03-22 | 2013-07-17 | 上海京海（安徽）化工有限公司 | Production method for high-content insoluble sulfur |
| CN103318848A (en) * | 2013-05-23 | 2013-09-25 | 上海京海（安徽）化工有限公司 | Production method of high-dispersion high-thermal-stability insoluble sulfur |
| CN104692337A (en) * | 2015-02-11 | 2015-06-10 | 上海京海（安徽）化工有限公司 | Insoluble sulfur capable of improving wear resistance of rubber products and preparation method thereof |
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