CN101486447B - Method for preparing insoluble sulfur and common sulfur powder by gasification continuous one-step water method - Google Patents
Method for preparing insoluble sulfur and common sulfur powder by gasification continuous one-step water method Download PDFInfo
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- CN101486447B CN101486447B CN2008102046150A CN200810204615A CN101486447B CN 101486447 B CN101486447 B CN 101486447B CN 2008102046150 A CN2008102046150 A CN 2008102046150A CN 200810204615 A CN200810204615 A CN 200810204615A CN 101486447 B CN101486447 B CN 101486447B
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Abstract
The invention relates to a method for preparing insoluble sulphur and common sulphur powder by continuous gasification one-step water method. After industrial grade sulphur is taken as raw material to generate sulphur vapour, quenching is carried out at the upper water layer of combined quenching liquid formed by water and carbon bisulfide; after quenching, most soluble sulphur enters the lower carbon bisulfide layer to form a carbon bisulfide solution containing soluble sulphur, the generated solid is the plastic mixture of insoluble sulphur and a small amount of soluble sulphur and deposits at the bottom of the carbon bisulfide layer; and then insoluble sulphur and the common sulphur powder are prepared respectively. The method is characterized by safety, environmental protection, high quality and being economical.
Description
Technical field
The invention belongs to the fine chemical technology field, be specifically related to the method that the industrial sulfury continuous one-step of a kind of usefulness water law prepares insoluble sulfur and common SULPHUR POWDER.
Background technology
Insoluble sulfur is a kind of vulcanizer of excellent performance, have the rubber item of making or surface of semi-finished no blooming, increase adhesive effect, particularly in the steel wire radial-ply tyre, can increase substantially the bond properties of rubber and steel wire, also help and improve operating environment; It also is a kind of good thiofide simultaneously, and vulcanization rate is accelerated, and sulfuration is even, and present domestic every year also must a large amount of import insoluble sulfur products.
The Manufacture of insoluble sulphur method is a lot, comprises contact process, evaporating method (dividing two step of high temperature water law and one step of high temperature dithiocarbonic anhydride method), low temperature liquid polymerization process etc.
China Granted publication CN100427386C discloses a kind of preparation method and production unit thereof of middle grade insoluble sulphur, with industrial sulphur and one package stabilizer is raw material, carry out polyreaction after low temperature (the sulphur liquid about the 300 ℃) fusion, grade insoluble sulphur in the production is the low temperature liquid polymerization process production technique.To be that the turnover ratio of insoluble sulfur is low have only about 40% the shortcoming of this technology, and economy is relatively poor, and the per-cent that present annual production accounts for domestic insoluble sulfur production is very low.
China Granted publication CN1270966C discloses the method that a kind of single stage method is made insoluble sulfur, industrial sulphur is carried out fusion, be fused into the liquid gaseous sulfur at 500～700 ℃, in dithiocarbonic anhydride, quench, be one step of high temperature dithiocarbonic anhydride method production technique, the quality product of production can reach the requirement of imported product.Because dithiocarbonic anhydride is inflammable, explosive liquid, directly the security that high temperature sulphur is fed in the dithiocarbonic anhydride liquid is worthy of consideration among this preparation technology, so that the insoluble sulfur annual production of this explained hereafter at present accounts for the per-cent of domestic production total amount is also little.
It is two step of high temperature water law that commonly used in the domestic production at present, turnout accounts for the preparation technology of domestic production total amount more than 60%:
As Fig. 1 is the process flow sheet of two step of high temperature water law, at 120～160 ℃ industrial sulphur is fused into liquid-state sulfur, generate about 600 ℃ sulphur steam by the tube furnace heating again, sulphur steam quenches in comprising the aqueous solution of stablizer, make the insoluble sulfur crude product of content about 60% through the first step compressing tablet, depickling, drying, pulverizing, extract with dithiocarbonic anhydride through second step again, make the insoluble sulfur of content 〉=90%, carry out the oil-filled type insoluble sulfur of oil-filled acquisition product at last.
The advantage of this technology is that security is good, continuous production, the transformation efficiency height of insoluble sulfur, steady quality.But shortcoming is that two step method production technique circuit is long, and the depickling step is washed in the requirement that quality product (thermostability, dispersiveness, fineness) does not reach imported product in addition, produces water and pollutes, and the environment friendliness is poor.
To sum up several preparation technologies, all both advantageous and disadvantageous, be difficult to various sets of advantages, although insoluble sulfur has the production history in more than 30 year at home, but also do not have one seat at present in the international market, the annual requirement that the domestic market is more than 30,000 ton is also occupied by imported product about half.A bit be in addition: which kind of technology no matter at present domestic is, the unconverted sulphur of 40% (low temperature is molten every method 60%), because of the reason of color and hardness can't be handled, can only buy the manufacturer of sulfuric acid and dithiocarbonic anhydride as sulfur waste sulphur, the utilization ratio of raw material sulphur is not high.
Summary of the invention
Technical problem to be solved of the present invention be to provide a kind of quality can reach the imported product requirement, safe, pollution-free, the gasification continuous one-step water law prepares the method for insoluble sulfur and common SULPHUR POWDER cheaply.
The present invention solves the problems of the technologies described above the technical scheme of taking: a kind of gasification continuous one-step water law prepares the method for insoluble sulfur and common SULPHUR POWDER, industrial sulphur is fused into liquid-state sulfur, generate sulphur steam by the tube furnace heating again, contain the insoluble sulfur about 60% in the sulphur steam, residue is soluble sulfur, wherein, with sulphur steam is raw material, constitute the associating hardening liquid with upper aqueous layer and lower floor's curing carbon-coating, quench in the upper aqueous layer with sulphur steam feeding associating hardening liquid earlier, the most of soluble sulfur in back that quenches enters and forms the dithiocarbonic anhydride solution that contains soluble sulfur in lower floor's curing carbon-coating, the solid that generates is the plastic mixture of insoluble sulfur and a small amount of soluble sulfur, is deposited on curing carbon-coating bottom; Prepare insoluble sulfur and common SULPHUR POWDER more respectively, comprising:
The preparation of A, insoluble sulfur:
The upper aqueous layer of separating the associating hardening liquid earlier, separate the dithiocarbonic anhydride solution that lower floor contains soluble sulfur again, add stablizer in the insoluble sulfur after separation and the plastic mixture of soluble sulfur, be cured processing, with the soluble sulfur in the extraction with carbon disulfide mixture, insoluble sulfur is crushed to the fineness of requirement through flushing, separation, dry, discharging, makes the high content insoluble sulfur powder; Or further carry out the oil-filled oil-filled type insoluble sulfur product made from naphthenic oil;
The preparation of B, common SULPHUR POWDER: the dithiocarbonic anhydride solution that will the contain soluble sulfur distillation dithiocarbonic anhydride of heating while stirring in still kettle, dithiocarbonic anhydride obtains light yellow sulphur crystal after reclaiming and finishing, and makes common SULPHUR POWDER after the pulverizing.
The effect that upper aqueous layer and lower floor curing carbon-coating constitute associating hardening liquid be by most heat in the water layer absorption sulphur steam and with in the physical method for separation water layer as the mineral ion of stablizer.
On the basis of such scheme, the dithiocarbonic anhydride that the extraction soluble sulfur is used is that the dithiocarbonic anhydride solution that will contain soluble sulfur distills the dithiocarbonic anhydride that reclaim the back.
The dithiocarbonic anhydride solution that contains soluble sulfur can also can produce in the extraction with carbon disulfide insoluble sulfur producing in sulphur steam quenching process, can be used to prepare common SULPHUR POWDER in the lump.
On the basis of such scheme, refer to 24 hours continuous production of insoluble sulfur continuously, adopt at least three jar continuous production, sulphur steam quenches in jar in turn, and what add the associating hardening liquid in the curing of insoluble sulfur, extraction, drying, discharging and the jar again is no more than 16 hours total time.
Concrete, adopting three jar continuous production, sulphur steam quenched in jar in per 8 hours in turn, and the time of each jar quenching is 8 hours; Adopt four jar continuous production, sulphur steam quenched in jar in per 6 hours in turn, and the time of each jar quenching is 6 hours; Adopt six jar continuous production, sulphur steam quenched in jar in per 4 hours in turn, and the time of each jar quenching is 4 hours.
The present invention has following three principal features:
A, quenching:
Quenching in the past or carry out in dithiocarbonic anhydride, or carry out in water all has shortcoming, the present invention to adopt sulphur steam to quench in the associating hardening liquid that water and dithiocarbonic anhydride are formed, and has removed the shortcoming of the two, combines the advantage of the two.
B, serialization:
At present domestic have only the first step of high temperature water law to realize continuous production, the thinking of domestic serialization research is the same with the first step in the high temperature water law, front end is a continuous quenching, the rear end is that the insoluble sulfur product comes out continuously, but because solidify in producing, time of flushing, dry, time that discharging needs and insoluble sulfur quenching and not matching, this idea is unrealistic, and does not temporarily have example at present.
And at least three jars of utilization of the present invention carry out alternate turns and use, really realize 24 hours continuously.
The utilization of C, unconverted sulphur:
Unconverted sulphur was all handled by sulfur waste sulphur in the technology in the past, possible reason is: obtain dark and hard sulfur waste sulphur sheet is thought to produce insoluble sulfur and certainly led to, be and the diverse product of sulphur raw material, color may be that impurity such as the iron filings brought into by environment in producing in metal ion in the hardening liquid or two steps, earth produce, and nobody further analyzes reason; The price difference of sulphur raw material and insoluble sulfur is more than 10 times, and these sulfur waste sulphurs are little to the benefit influence, and in addition, the design of still kettle is fairly simple, does not need to stir, as long as a tube row is just passable except that the sulfur waste sulphur of liquid.
See that by the requirement of modern enterprise and the development of society the utilization ratio of raw material sulphur has only 60% (the watery fusion method has only 40%) in above-mentioned several technologies, is unfavorable for building a conservation-minded society.The technology that the present invention takes is to analyze the color of sulfur waste sulphur and hardness owing to sulphur after having distilled dithiocarbonic anhydride melts generation once more, therefore in treatment process, reduced the process that sulphur heats up once more and melts in the traditional technology, after having distilled dithiocarbonic anhydride, the sulphur sheet is directly emitted still kettle, obtain lurid sulphur crystal, make common SULPHUR POWDER after the pulverizing, really realize the utilization of raw material sulphur 100%.
The invention provides another kind of thinking, adopt duration control method to solve the continuous production problem, for example use the production of three jars, the cool time is 7～8 hours, solidified 3～5 hours, about 8 hours of flushing, dry, discharging add about 1 hour of entry and dithiocarbonic anhydride associating hardening liquid once more, and a jar can be finished in 24 hours once and produce, three jars switched once in per 8 hours, outside the time that deduction sulphur steam switches, realize 24 hours continuous quenchings, continuous production.Be to curing, flushing, drying, discharging and add entry once more and dithiocarbonic anhydride associating hardening liquid 2 hours time of increase with 4 jar purposes.
The present invention specifically is achieved like this, and it mainly may further comprise the steps:
1, molten sulphur: be 120 ℃～160 ℃ in temperature industrial sulphur is fused into liquid-state sulfur;
2, sulphur gasification: liquid-state sulfur adds thermogenesis sulphur steam by tube furnace;
3, quench: the difference (water: 1 that utilizes density, dithiocarbonic anhydride: 1.26, sulphur: 2.06), constitute the associating hardening liquid with upper aqueous layer and lower floor's curing carbon-coating, quench in the upper aqueous layer with sulphur steam feeding associating hardening liquid, the most of soluble sulfur in back that quenches enters and forms the dithiocarbonic anhydride solution that contains soluble sulfur in lower floor's curing carbon-coating, and the solid of generation is the plastic mixture of insoluble sulfur and a small amount of soluble sulfur, is deposited on curing carbon-coating bottom;
4, the preparation of insoluble sulfur: the upper aqueous layer of separating the associating hardening liquid earlier, water must separate fully, may take away a spot of dithiocarbonic anhydride in the water, sink to basin bottom, available submersible pump is returned dithiocarbonic anhydride groove jar, separate the dithiocarbonic anhydride solution that lower floor contains soluble sulfur again, add stablizer in the insoluble sulfur after separation and the plastic mixture of soluble sulfur, be cured processing, use dithiocarbonic anhydride solvent extraction soluble sulfur wherein then, through flushing, separate, drying is made the high content insoluble sulfur powder, be crushed to the fineness of requirement, further carry out the oil-filled oil-filled type insoluble sulfur product made from naphthenic oil;
5, the preparation of the recycling of dithiocarbonic anhydride and common SULPHUR POWDER: the dithiocarbonic anhydride solution that contains soluble sulfur that produces in quenching and the flushing process, dithiocarbonic anhydride is reclaimed in the evaporation of heating, dithiocarbonic anhydride obtains light yellow sulphur crystal after reclaiming fully, makes common SULPHUR POWDER after the pulverizing.
6, in the above-mentioned associating hardening liquid, be added with stablizer in the upper aqueous layer;
7, water layer has outlet valve of a water intaking valve in the quenching jar, and purpose is that the temperature of control water is no more than 42 ℃.
The invention has the beneficial effects as follows:
1, the present invention helps to break external monopolization to high quality insoluble sulphur, the level that process safety is good, the transformation efficiency height of insoluble sulfur, continuous production, quality can reach imported product, improved utilization ratio of raw materials simultaneously, the former part that is used as sulfur waste sulphur is used to prepare common SULPHUR POWDER, turns waste into wealth;
2, insoluble sulfur is the porous crystal sulphur that gas quenching produces, common SULPHUR POWDER is the loose crystallization sulphur that distillation dithiocarbonic anhydride is directly separated out, be very easy to pulverize, particle dia can reach 10～30 μ m, reduced the energy consumption of pulverizing, solved the requirement of client insoluble sulfur and common SULPHUR POWDER fineness;
3, the present invention adopts water and the immiscible principle design quenching technology of dithiocarbonic anhydride, has reduced water-washing step, has avoided the pollution to environment, has reduced the content of the mineral ion in insoluble sulfur and the common SULPHUR POWDER simultaneously, has improved the dispersiveness of product;
4, stablizer of the present invention when quenching water layer adds, when solidifying, also added organic stabilizer, thereby improved the thermostability of insoluble sulfur, satisfied insoluble sulfur at 105 ℃ thermostability 〉=75% and in the requirement of 120 ℃ thermostability 〉=40%.
Description of drawings
Fig. 1 is the process flow sheet of high temperature two step method in the prior art.
Fig. 2 is the process flow sheet of gasification continuous one-step water law of the present invention.
Fig. 3-1～Fig. 3-4 is three jar quantity-produceds of embodiment of the invention schema.
Embodiment
Embodiment 1
A kind of gasification continuous one-step water law prepares the method for insoluble sulfur and common SULPHUR POWDER, be 120 ℃～160 ℃ in temperature industrial sulphur is fused into liquid-state sulfur, generate sulphur steam by the tube furnace heating again, contain the insoluble sulfur about 60% in the sulphur steam, residue is soluble sulfur, wherein, be raw material with sulphur steam, constitute the associating hardening liquid with upper aqueous layer and lower floor's curing carbon-coating.
Quench in the upper aqueous layer with sulphur steam feeding associating hardening liquid earlier, the most of soluble sulfur in back that quenches enters and forms the dithiocarbonic anhydride solution that contains soluble sulfur in lower floor's curing carbon-coating, the solid that generates is the plastic mixture of insoluble sulfur and a small amount of soluble sulfur, is deposited on curing carbon-coating bottom; Prepare insoluble sulfur and common SULPHUR POWDER more respectively, comprising:
The preparation of A, insoluble sulfur:
The upper aqueous layer of separating the associating hardening liquid earlier, separate the dithiocarbonic anhydride solution that lower floor contains soluble sulfur again, add stablizer in the insoluble sulfur after separation and the plastic mixture of soluble sulfur, be cured processing, distill the soluble sulfur in the extraction with carbon disulfide mixture that reclaims the back with the dithiocarbonic anhydride solution that contains soluble sulfur, insoluble sulfur is crushed to the fineness of requirement through flushing, separation, dry, discharging, makes the high content insoluble sulfur powder; Or further carry out the oil-filled oil-filled type insoluble sulfur product made from naphthenic oil, wherein, the dithiocarbonic anhydride that the extraction soluble sulfur is used is that the dithiocarbonic anhydride solution that will contain soluble sulfur distills the dithiocarbonic anhydride that reclaim the back;
The preparation of B, common SULPHUR POWDER: the dithiocarbonic anhydride solution that contains soluble sulfur that will in sulphur steam quenching and insoluble sulfur flushing process, the produce distillation dithiocarbonic anhydride of in still kettle, heating while stirring, after dithiocarbonic anhydride reclaims and finishes, obtain light yellow sulphur crystal, make common SULPHUR POWDER after the pulverizing.
The effect that upper aqueous layer and lower floor curing carbon-coating constitute associating hardening liquid be by most heat in the water layer absorption sulphur steam and with in the physical method for separation water layer as the mineral ion of stablizer.
24 hours continuous production of insoluble sulfur adopt three jar continuous production, and sulphur steam quenched in three jars in per 8 hours in turn:
As Fig. 3-1: sulphur steam feeds in the upper aqueous layer of the associating hardening liquid in jar 1 and quenches, and the cool time is 8 hours;
As Fig. 3-2: sulphur steam feeds in jars 2 and quenched 8 hours, and carries out curing, the flushing of insoluble sulfur in jar 1;
As Fig. 3-3: sulphur steam feeds in jars 3 and quenched 8 hours, separates in jar 1, dry, discharging and add associating hardening liquid once more, and carries out curing, the flushing of insoluble sulfur again in the jar 2;
As Fig. 3-4: sulphur steam feeds in jar 1 and quenched 8 hours, separates in jar 2, dry, discharging and add associating hardening liquid once more, and carries out curing, the flushing of insoluble sulfur again in the jar 3.
So carry out serialization production.
Embodiment 2
The production principle of four jars of the present invention is identical with three jars, and just the time of quenching is 6 hours, for curing, flushing, drying, the discharging of insoluble sulfur and add entry once more and the process of dithiocarbonic anhydride associating hardening liquid in increased by 2 hours time.
Claims (3)
1. a gasification continuous one-step water law prepares the method for insoluble sulfur and common SULPHUR POWDER, industrial sulphur is fused into liquid-state sulfur, generate sulphur steam by the tube furnace heating again, it is characterized in that: with sulphur steam is raw material, constitute the associating hardening liquid with upper aqueous layer and lower floor's curing carbon-coating, quench in the upper aqueous layer with sulphur steam feeding associating hardening liquid earlier, the most of soluble sulfur in back that quenches enters and forms the dithiocarbonic anhydride solution that contains soluble sulfur in lower floor's curing carbon-coating, the solid that generates is the plastic mixture of insoluble sulfur and a small amount of soluble sulfur, is deposited on curing carbon-coating bottom; Prepare insoluble sulfur and common SULPHUR POWDER more respectively, comprising: the preparation of A, insoluble sulfur:
The upper aqueous layer of separating the associating hardening liquid earlier, separate the dithiocarbonic anhydride solution that lower floor contains soluble sulfur again, add stablizer in the insoluble sulfur after separation and the plastic mixture of soluble sulfur, be cured processing, with the soluble sulfur in the extraction with carbon disulfide mixture, insoluble sulfur is pulverized and is made the high content insoluble sulfur powder through flushing, separation, dry, discharging; Or further carry out the oil-filled oil-filled type insoluble sulfur product made from naphthenic oil;
The preparation of B, common SULPHUR POWDER:
The dithiocarbonic anhydride solution that will the contain soluble sulfur distillation dithiocarbonic anhydride of heating while stirring in still kettle, dithiocarbonic anhydride obtains light yellow sulphur crystal after reclaiming and finishing, and makes common SULPHUR POWDER after the pulverizing.
2. gasification continuous one-step water law according to claim 1 prepares the method for insoluble sulfur and common SULPHUR POWDER, it is characterized in that: the dithiocarbonic anhydride that the extraction soluble sulfur is used comprises that the dithiocarbonic anhydride solution that will contain soluble sulfur distills the dithiocarbonic anhydride that reclaim the back.
3. gasification continuous one-step water law according to claim 1 and 2 prepares the method for insoluble sulfur and common SULPHUR POWDER, it is characterized in that: adopt at least three jar continuous production, sulphur steam quenches in jar in turn, and what add the associating hardening liquid in the curing of insoluble sulfur, extraction, drying, discharging and the jar again is no more than 16 hours total time.
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| CN102009962B (en) * | 2010-12-22 | 2012-09-05 | 江西恒兴源化工有限公司 | Process for continuously producing insoluble sulfur by pipeline |
| CN102167292B (en) * | 2011-02-01 | 2012-07-18 | 无锡华盛橡胶新材料科技股份有限公司 | Equipment and method for producing medium-grade insoluble sulfur with continuous ageing method |
| CN102511496B (en) * | 2011-10-25 | 2013-12-25 | 许惠朝 | Method for preparing hydrophilic ultrafine sulfur powder |
| CN102674265A (en) * | 2012-05-28 | 2012-09-19 | 吴勇 | Method for producing insoluble sulfur by one-step water method |
| CN105502304A (en) * | 2016-01-22 | 2016-04-20 | 上海京海（安徽）化工有限公司 | Preparation method of energy-saving and environment-friendly insoluble sulfur |
| CN108203081B (en) * | 2018-03-19 | 2023-09-01 | 无锡华盛橡胶新材料科技股份有限公司 | Production method and production equipment of oil-filled insoluble sulfur |
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| CN101066753A (en) * | 2007-05-29 | 2007-11-07 | 谭建中 | Continuous one-step process for producing insoluble sulphur |
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