CN102145878A - Method for continuously preparing poly-sulphur - Google Patents
Method for continuously preparing poly-sulphur Download PDFInfo
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- CN102145878A CN102145878A CN2010190870225A CN201019087022A CN102145878A CN 102145878 A CN102145878 A CN 102145878A CN 2010190870225 A CN2010190870225 A CN 2010190870225A CN 201019087022 A CN201019087022 A CN 201019087022A CN 102145878 A CN102145878 A CN 102145878A
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Abstract
The invention relates to a method for preparing poly-sulphur, in particular to a method for continuously preparing the poly-sulphur, which comprises the following steps of: heating and warming up raw material sulphur; carrying out shock cooling on the high temperature sulphur and a mixed solvent and simultaneously carrying out rotary primary curing on the high temperature sulphur; carrying out transfer; carrying out secondary curing; carrying out filtering, collection and washing by a disk multifunctional device; carrying out spiral vacuum drying; and carrying out grinding, sieving and oil charging. The method for continuously preparing the poly-sulphur is characterized in that the method for continuously preparing the poly-sulphur comprises the following steps that: a), solid or liquid sulphur is heated to the temperature of 580 to 690 DEG C and the high-temperature sulphur sent out from a heater and the mixed solvent sent out from a circulating tank are subjected to shock cooling in a mass ratio of 1:10-20 in a synthesizer; and b), a quenched solid and liquid mixture continuously enters a primary curing device which always rotates and continuously enters a transfer tank from the lower end of the primary curing device. The method for continuously preparing the poly-sulphur has low energy consumption, high safety factor and no pollution to the environment and can be used for continuously preparing uniform and high-quality poly-sulphur products and the like.
Description
Technical field
The present invention relates to a kind of method for preparing polymerised sulphur, comprise raw material sulphur heat temperature raising; The mixed solvent quenching of high temperature sulphur (promptly quenching) is rotated one-step solidification simultaneously; Transfer; Regelate; The multi-functional device of disc type filters, collects, washs; Spiral vacuum-drying; Pulverizing, screening, oil-filled are specially a kind of continuous method for preparing polymerised sulphur.
Background technology
Along with the fast development of radial industry, the demand of its widely used vulcanizing agent---high quality polymerised sulphur is also increasing.Therefore, the production method of polymerised sulphur had also obtained fast development in recent years.The patent No. is that 03117763.8 disclosed method is to use special mixing tank and multi-functional dry machine to realize single stage method production polymerised sulphur.Its shortcoming is: this method is produced discontinuous, belongs to batch production, and single batch of product production is little, and quality is influenced greatly by manual operation.And for example the patent No. is that 200710105733 disclosed methods are distance method in the closed tin to be changed into opening wide under the water seal carry continuous processing in the solvent trough, its shortcoming is: dithiocarbonic anhydride flash-point and boiling point are very low, constantly flowing and spraying into continuously under the state of high temperature sulphur, dithiocarbonic anhydride is easily by emerging and contaminate environment and generation security incident in the water.
Summary of the invention
The present invention provides a kind of and can realize that energy expenditure is less, safety coefficient is higher in the even high-quality polymerised sulphur of airtight, continuous preparation just at above technical problem, and a kind of continuous method for preparing polymerised sulphur that environment is not polluted.
Concrete technical scheme of the present invention is as follows:
A kind of continuous method for preparing polymerised sulphur may further comprise the steps:
A) with solid-state or liquid-state sulfur, make it heat to 580～690 ℃, by the high temperature sulphur of sending in the well heater and by the mixed solvent of sending in the circulation tank according to 1: 10～20 mass ratio quenchings in synthesizer (promptly quench), dithiocarbonic anhydride and unsaturated olefin mixed solvent temperature are controlled at 40～60 ℃;
B) the solid, liquid mixture after the quenching constantly enters the one-step solidification device of rotation all the time, and constantly enters the transfer jar by one-step solidification device lower end;
C) agitator one that is fixed in the transfer jar and imports one-step solidification device lower end is with the continuous material copy of speed of one-step solidification device rotation, constantly entered in the transfer jar that is constantly stirred by agitator two by the material of one-step solidification in the one-step solidification device, the mixture in the transfer jar enters the regelate device;
D) in the regelate device solid materials by sedimentation, the partially liq material enters circulation tank together with the fresh dithiocarbonic anhydride of being sent by pure dithiocarbonic anhydride hold-up vessel, add unsaturated olefin in proportion after circulate behind heat exchanger two temperature controls, solids strip liquid heats up and stirs curing by agitator three, mixture after the curing enters the multi-functional device of disc type and filters, under the promotion that material is scraped in the multi-functional device of disc type, solid materials after the filtration is sent to the multi-functional device washing section of disc type, and the pure dithiocarbonic anhydride of being sent here by pure dithiocarbonic anhydride hold-up vessel constantly washs;
E) the high purity polymerised sulphur solid after the washing enters spiral dryer one drying, and the material of being exported by spiral dryer one middle outlet enters in the spiral dryer two;
F) the isolated dithiocarbonic anhydride liquid that contains unconverted sulphur and unsaturated olefin enters distillation tower in filtration, the washing process, the fresh dithiocarbonic anhydride that distills out all enters pure dithiocarbonic anhydride hold-up vessel after heat exchanger one cools off after heat exchanger three coolings and by the carbon disulfide gas that spiral dryer one and spiral dryer two vacuum are extracted out, dithiocarbonic anhydride is recovered and recycles, and unconverted sulphur and a small amount of unsaturated olefin get byproduct through thawing, cooling, film-making;
G) dried high purity polymerised sulphur gets final polymerised sulphur product after pulverizing, screening, oil-filled system are handled.
Positively effect of the present invention shows: energy expenditure is less, safety coefficient is higher, environmentally safe and can prepare uniform, high-quality polymerised sulphur product continuously.
Description of drawings
Fig. 1 is a synoptic diagram of the present invention
Wherein, 1---well heater, 2---synthesizer, 3---one-step solidification device, 4---agitator one, 5---transfer jar, 6---agitator two, 7---regelate device, 8---the multi-functional device of disc type, 9---material scrape, 10---spiral dryer one, 11---spiral dryer two, 12---pulverizing, screening, oil-filled system, 13---heat exchanger one, 14---circulation tank, 15---heat exchanger two, 16---pure dithiocarbonic anhydride hold-up vessel, 17---heat exchanger three, 18---distillation tower, 19---agitators three.
Embodiment
The invention will be further described below in conjunction with embodiment and Figure of description
Embodiment
Preferred purity is the solid-state or liquid-state sulfur more than 99.9%, be heated and be warmed up to 580～690 ℃, with mass ratio is that 98.0～99.9: 0.1～2.0 dithiocarbonic anhydride and unsaturated olefin mixed solvent temperature are controlled at 40～60 ℃, by in the well heater with 800～1000 kilograms of/hour high temperature sulphur of sending and by in the circulation tank with 8000～20000 kilograms of/hour mixed solvent of sending quenchings in synthesizer (promptly quenching); Mixture after the quenching constantly enters in the one-step solidification device, keep of the speed rotation of the one-step solidification device of tilting band material lifting flights with per minute 0.1～3.0 circle, keep one-step solidification device liquid level 100～500mm under its opening for feed position simultaneously, solid materials after keeping quenching is in the liquid material all the time, and under material lifting flights promotes, constantly slowly transmit to one-step solidification device lower end, material by one-step solidification device upper end in the process that transmit the lower end by one-step solidification, when material arrives one-step solidification device lower end, the agitator one that is fixed in the transfer jar and imports one-step solidification device lower end is constantly entered in the transfer jars that constantly stirred by agitator two by the material of one-step solidification in the one-step solidification device with the continuous material copy of speed of one-step solidification device rotation; Mixture constantly enters in the regelate device under agitator two stirs in the transfer jar; Solid materials is by sedimentation in the regelate device, the partially liq material enters circulation tank together with the fresh dithiocarbonic anhydride of being sent by pure dithiocarbonic anhydride hold-up vessel, add unsaturated olefin in proportion after circulate behind over-heat-exchanger two temperature controls, when computable solid materials quality reaches more than 5000 kilograms in the regelate device, begin to be with liquid to stir the curing that heats up, solidification value be controlled at 50～90 ℃ 1～3 hour, in order to realize the continuity of technology, the regelate device should be provided with 2 at least; Mixture after the curing constantly enters filtrating area filtration in the multi-functional device of disc type, under the promotion that material is scraped in the multi-functional device of disc type, solid materials after the filtration is sent to the multi-functional device washing section of disc type, and the pure dithiocarbonic anhydride of being sent here by pure dithiocarbonic anhydride hold-up vessel constantly washs, after the washing, polymerised sulphur purity reaches more than 94%; Under the promotion that material is scraped in the multi-functional device of disc type, the high purity polymerised sulphur by vacuum suction filter after the washing is carried a small amount of dithiocarbonic anhydride (10～20%) secretly and is entered spiral dryer one, and constantly in spiral dryer one, evenly copy by spiral, feed 50～90 ℃ of circulating hot waters at spiral dryer one chuck simultaneously, vacuum tightness is 0.06～0.15MPa in the control spiral dryer one, constantly aspirate the carbon disulfide gas that is evaporated in the spiral dryer one, regulate and fixing revolution speed of screw in the spiral dryer one, dithiocarbonic anhydride mass ratio in the control spiral dryer one discharge port polymerised sulphur is less than 5%, material by the output of spiral dryer one middle outlet enters in the spiral dryer two, working method and spiral dryer one are similar, and control spiral dryer two discharge port dithiocarbonic anhydride mass ratioes are less than 0.5%; Be admitted in the distillation tower and distill by filtration in the multi-functional device of disc type, the isolated mixing solutions that contains soluble sulfur of washing, the fresh dithiocarbonic anhydride that distills out all enters pure dithiocarbonic anhydride hold-up vessel after heat exchanger one cools off after heat exchanger three coolings and by the carbon disulfide gas that spiral dryer one and spiral dryer two vacuum are extracted out, soluble sulfur and a small amount of unsaturated olefin get byproduct through thawing, cooling, film-making; The pulverizing of high purity polymerised sulphur solid process, screening, oil-filled system by spiral dryer two outlet outputs get final polymerised sulphur product after handling.
Claims (6)
1. method for preparing continuously polymerised sulphur is characterized in that may further comprise the steps:
A) with solid-state or liquid-state sulfur, make it heat to 580～690 ℃, by the high temperature sulphur of sending in the well heater and by the mixed solvent of sending in the circulation tank according to 1: 10～20 mass ratio quenchings in synthesizer (promptly quench), dithiocarbonic anhydride and unsaturated olefin mixed solvent temperature are controlled at 40～60 ℃;
B) the solid, liquid mixture after the quenching constantly enters the one-step solidification device of rotation all the time, and constantly enters the transfer jar by one-step solidification device lower end;
C) agitator one that is fixed in the transfer jar and imports one-step solidification device lower end is with the continuous material copy of speed of one-step solidification device rotation, constantly entered in the transfer jar that is constantly stirred by agitator two by the material of one-step solidification in the one-step solidification device, the mixture in the transfer jar enters the regelate device;
D) in the regelate device solid materials by sedimentation, the partially liq material enters circulation tank together with the fresh dithiocarbonic anhydride of being sent by pure dithiocarbonic anhydride hold-up vessel, add unsaturated olefin in proportion after circulate behind heat exchanger two temperature controls, solids strip liquid heats up and stirs curing by agitator three, mixture after the curing enters the multi-functional device of disc type and filters, under the promotion that material is scraped in the multi-functional device of disc type, solid materials after the filtration is sent to the multi-functional device washing section of disc type, and the pure dithiocarbonic anhydride of being sent here by pure dithiocarbonic anhydride hold-up vessel constantly washs;
E) the high purity polymerised sulphur solid after the washing enters spiral dryer one drying, and the material of being exported by spiral dryer one middle outlet enters in the spiral dryer two;
F) the isolated dithiocarbonic anhydride liquid that contains unconverted sulphur and unsaturated olefin enters distillation tower in filtration, the washing process, the fresh dithiocarbonic anhydride that distills out all enters pure dithiocarbonic anhydride hold-up vessel after heat exchanger one cools off after heat exchanger three coolings and by the carbon disulfide gas that moisture eliminator one and moisture eliminator two vacuum are extracted out, dithiocarbonic anhydride is recovered and recycles, and unconverted sulphur and a small amount of unsaturated olefin get byproduct through thawing, cooling, film-making;
G) dried high purity polymerised sulphur gets final polymerised sulphur product after pulverizing, screening, oil-filled system are handled.
2. a kind of continuous method for preparing polymerised sulphur according to claim 1, it is characterized in that: the mixed solvent among the step a is dithiocarbonic anhydride and unsaturated olefin.
3. a kind of continuous method for preparing polymerised sulphur according to claim 1, it is characterized in that: the one-step solidification device is tilting and is with material lifting flights, speed of rotation is per minute 0.1～3 circle, one-step solidification device solid materials is to be transmitted to the bottom by top together with liquid material under the promotion of material lifting flights, and in transmittance process, carry out one-step solidification, one-step solidification device liquid level remains on 100～500mm under its opening for feed position, and solid materials is submerged in the liquid material all the time.
4. a kind of continuous method for preparing polymerised sulphur according to claim 1, it is characterized in that: the regelate device constantly receives from the solid materials in the transfer jar, it is 50～90 ℃ that solids strip liquid stirs solidification value, be 1～3 hour set time, and the quantity of regelate device setting is more than 2 or 2.
5. a kind of continuous method for preparing polymerised sulphur according to claim 1, it is characterized in that: the mass ratio that the solid materials that enters helicoid screw dryer one contains dithiocarbonic anhydride is 10～20%, solid materials is evenly copied by spiral in spiral dryer one, the chuck circulating hot water temperature of spiral dryer one is 70～90 ℃, and vacuum tightness is 0.06～0.15MPa in the spiral dryer one.
6. a kind of continuous method for preparing polymerised sulphur according to claim 1 is characterized in that: the mass ratio that solid materials contains dithiocarbonic anhydride behind the primary drying is less than 5%, and solid materials contains the mass ratio of dithiocarbonic anhydride less than 0.5% after the redrying.
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| CN 201019087022 CN102145878B (en) | 2010-02-08 | 2010-02-08 | Method for continuously preparing poly-sulphur |
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| CN 201019087022 CN102145878B (en) | 2010-02-08 | 2010-02-08 | Method for continuously preparing poly-sulphur |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961105A (en) * | 2015-07-02 | 2015-10-07 | 山东阳谷华泰化工股份有限公司 | Continuous curing method for insoluble sulfur |
| CN106395757A (en) * | 2016-03-02 | 2017-02-15 | 赵水斌 | Fully-automatic continuous production method for insoluble sulfur |
| CN112694065A (en) * | 2021-01-29 | 2021-04-23 | 华油惠博普科技股份有限公司 | Crude sulfur dehydration purification process and device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2107657C1 (en) * | 1997-04-11 | 1998-03-27 | Вячеслав Александрович Чиндяскин | Method of production of insoluble sulfur and device for its embodiment |
| WO2002000549A1 (en) * | 2000-06-28 | 2002-01-03 | Ege Kimya Sanayi Ve Ticaret A.S. | A process for the production of polymeric allotropes of sulfur |
| CN101066753A (en) * | 2007-05-29 | 2007-11-07 | 谭建中 | Continuous one-step process for producing insoluble sulphur |
| CN101343045A (en) * | 2008-08-26 | 2009-01-14 | 山东省单县化工有限公司 | Method for continuous preparation of sulfur with high heat-stability and insolubility |
-
2010
- 2010-02-08 CN CN 201019087022 patent/CN102145878B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2107657C1 (en) * | 1997-04-11 | 1998-03-27 | Вячеслав Александрович Чиндяскин | Method of production of insoluble sulfur and device for its embodiment |
| WO2002000549A1 (en) * | 2000-06-28 | 2002-01-03 | Ege Kimya Sanayi Ve Ticaret A.S. | A process for the production of polymeric allotropes of sulfur |
| CN101066753A (en) * | 2007-05-29 | 2007-11-07 | 谭建中 | Continuous one-step process for producing insoluble sulphur |
| CN101343045A (en) * | 2008-08-26 | 2009-01-14 | 山东省单县化工有限公司 | Method for continuous preparation of sulfur with high heat-stability and insolubility |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961105A (en) * | 2015-07-02 | 2015-10-07 | 山东阳谷华泰化工股份有限公司 | Continuous curing method for insoluble sulfur |
| CN104961105B (en) * | 2015-07-02 | 2018-02-23 | 山东阳谷华泰化工股份有限公司 | A kind of serialization ageing method of insoluble sulfuy |
| CN106395757A (en) * | 2016-03-02 | 2017-02-15 | 赵水斌 | Fully-automatic continuous production method for insoluble sulfur |
| CN112694065A (en) * | 2021-01-29 | 2021-04-23 | 华油惠博普科技股份有限公司 | Crude sulfur dehydration purification process and device |
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| CN102145878B (en) | 2013-04-03 |
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