CN101081715B - Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process - Google Patents
Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process Download PDFInfo
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- CN101081715B CN101081715B CN200710027443XA CN200710027443A CN101081715B CN 101081715 B CN101081715 B CN 101081715B CN 200710027443X A CN200710027443X A CN 200710027443XA CN 200710027443 A CN200710027443 A CN 200710027443A CN 101081715 B CN101081715 B CN 101081715B
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Abstract
The present invention is process of treating mother liquid residue from sodium formate method to produce sodium hyosulfate and after being rectified to recover methanol. The process includes the following steps: 1. concentrating to obtain concentrated residue with or without sodium formate recovery; 2. incinerating the concentrated residue in a converter or one combined furnace to obtain incinerated clinker; 3. discharging high temperature clinker; 4. dissolving the clinker to form water solution; 5. absorbing SO2 from the incinerating fume with the water solution; and 6. adding sulfur to theabsorbed solution to prepare sodium thiosulfate. The process can eliminate pollutant while producing sodium thiosulfate as chemical material.
Description
Affiliated technical field
The present invention relates to a kind of sodium formate method and produce the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, be particularly related to a kind of methanol rectified raffinate or its enriched material that produces in the high temperature incineration processing production process that adopt, and utilize the incineration residue lysate to absorb a large amount of sulfurous gas that burning process produces, incineration residue and flue gas all are effectively addressed and reclaim the method for Sulfothiorine.
Background technology
V-Brite B (Sodium dithionite or Sodium hydrosulfite) popular name vat powder, it is industrial reductive agent commonly used, mainly as fabrics printing and dyeing and papermaking bleaching.Make raw material with sodium formiate, Sodium Pyrosulfite and sulfurous gas in the V-Brite B production, make solvent, add oxyethane in the production process with methyl alcohol, about 80 ℃ of temperature, the synthetic V-Brite B of intermittent type batch reaction under the non-pressurized condition.Its synthesis mother liquid needs to handle.The treating processes of synthesis mother liquid is that S-WAT is reclaimed in neutralization earlier, and methyl alcohol is reclaimed in rectifying again.The rectifier bottoms that reclaims methyl alcohol in rectifying can produce distillation residual liquid.Distillation residual liquid contains the inorganic and organic sulfocompound that the sodium formiate of complete reaction not, the S-WAT that does not reclaim fully, methyl alcohol, side reaction produce, and its chemical oxygen demand (COD value) is up to every liter more than tens0000 milligrams.One ton of V-Brite B of every production will be discharged COD more than 100 kilograms from distillation residual liquid.Because of the COD concentration height of distillation residual liquid, quantity is big, contains a large amount of organic sulfides again, as not handling direct discharging, can cause serious environmental to pollute.
Distillation residual liquid contains the inorganic and organic sulfide that in a large number bacterium is had the ability of killing, so be difficult to handle with the method for biochemical treatment.
With the method for oxygenant chemical oxidation, although feasible technically, because of flow process is longer, the intermediate product complexity, COD is difficult to up to standard, and processing cost is higher.
Burning is economically viable method, but garbage combustion device commonly used can produce the SO that contains high density in burning process
2With malodorous flue gas, and can produce alkaline waste material, secondary pollution is big, so general waste incineration field is extremely difficult.
Summary of the invention
The defective and the deficiency that the objective of the invention is to exist at above-mentioned prior art provide a kind of sodium formate method to produce the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, this method can not only be eliminated environmental pollution, and can obtain industrial chemicals-Sulfothiorine.
For achieving the above object, the invention provides a kind of treatment process with the raffinate behind the mother liquor rectifying recovery methyl alcohol in the process of sodium formate method production V-Brite B, it is characterized in that, comprise the steps: step 1, produce in the V-Brite B process at sodium formate method, the raffinate that raffinate behind the methyl alcohol concentrates after obtaining concentrated residue or will mother liquor rectifying reclaiming methyl alcohol is reclaimed in mother liquor rectifying obtain concentrated residue after reclaiming sodium formiate through concentrating; Step 2, in the combination stove of a section or two sections converters or converter and stationary furnace, adopt liquid or gas fuel combustion, when furnace temperature is raised to 600-1300 ℃, concentrated residue is sent in the converter continuously or intermittently, regulate the air capacity that feeds simultaneously, the burning concentrated residue obtains containing the incineration flue gas of sulfurous gas, keeps furnace temperature in the combustion processes at 600-1300 ℃; Step 3 stops concentrated residue being sent in the converter, keeps temperature in the converter, makes and burns the slag fusion, opens the drain hole of converter, and the burning slag of molten state is poured out; Step 4, blowing finishes, and closes drain hole, enters the operation of step 2 once more; Step 5 will be burned slag and will be dissolved into the aqueous solution, filter out insolubles then; Step 6, the incineration flue gas that burning concentrated residue in the step 2 obtains is sent in the tail gas washing tower, add the aqueous solution that obtains in an amount of step 5 in tail gas washing tower, the sulfurous gas in the incineration flue gas is absorbed the smoke absorption liquid that obtains containing Sulfothiorine and S-WAT; And step 7, the smoke absorption liquid in the step 6 is added in the retort, add sulphur, temperature reaction is filtered then, is concentrated, filtration, crystallization, centrifugal classification promptly get the Sulfothiorine finished product.
In the step 1, after distillation residual liquid concentrated, when reclaiming sodium formiate and be the crystal of main component, add methyl alcohol leaching, washing crystal, filter then, the crystal that leaches is used for the synthetic of V-Brite B.
Described converter is the structure of box hat inner lining refractory, drives converter with machinery and rotates around axis, and converter is spindle-type, and is small at both ends and big in the middle, and burner is equipped with heating unit, and the stove tail communicates with secondary combustion chamber or flue; Concentrated residue to be burned can add the bosh from burner or stove tail; Bosh has discharge port; Be used to emit the slag after the burning.
In step 3, when material in the converter reaches the 1/8-1/2 of furnace volume, stop into concentrated residue.
In step 3, keep the interior temperature of converter to be higher than the slag fusing point, best 750～900 ℃.
In step 6, incineration flue gas is sent into earlier in the one-level tail gas washing tower, adds the incineration residue lysate in the step 5 in the one-level tail gas washing tower, and spray absorbs sulfur in smoke, and incineration flue gas is discharging after the washing of secondary tail gas washing tower again.
The slag that obtains in step 3 is as the alkaline sodium salt byproduct.
From the above mentioned, the present invention carries out burning disposal with this kind distillation residual liquid (or its concentrated residue), and absorbs sulfurous gas in the incineration flue gas with the lysate of incineration residue, to remove smoke and the secondary pollution of incineration residue; And absorption liquid through adding sulphur, filtration, concentrate, operation such as crystallization handles the recyclable Sulfothiorine in back, reclaimed resource.Also the slag that obtains can be used for other industry as the alkaline sodium salt byproduct.
Description of drawings
Fig. 1 is one embodiment of the invention schema;
Fig. 2 is another embodiment of the present invention schema.
Embodiment
Sodium formate method of the present invention is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, comprises the steps:
Step 1 is produced in the V-Brite B process at sodium formate method, the raffinate behind the mother liquor rectifying recovery methyl alcohol is concentrated obtain concentrated residue or the raffinate behind the mother liquor rectifying recovery methyl alcohol is obtained concentrated residue after concentrating the recovery sodium formiate;
Step 2, in the combination stove of a section or two sections converters or converter and stationary furnace, adopt liquid or gas fuel combustion, when furnace temperature is raised to 600-1300 ℃, concentrated residue is sent in the converter continuously or intermittently, regulate the air capacity that feeds simultaneously, the burning concentrated residue obtains containing the incineration flue gas of sulfurous gas, keeps furnace temperature in the combustion processes at 600-1300 ℃;
Step 3 stops concentrated residue being sent in the converter, keeps temperature in the converter, makes and burns the slag fusion, opens the drain hole of converter, and the burning slag of molten state is poured out;
Step 4, blowing finishes, and closes drain hole, enters the operation of step 2 once more;
Step 5 will be burned slag and will be dissolved into the aqueous solution, filter out insolubles then;
Step 6, the incineration flue gas that burning concentrated residue in the step 2 obtains is sent in the tail gas washing tower, add the aqueous solution that obtains in an amount of step 5 in tail gas washing tower, the sulfurous gas in the incineration flue gas is absorbed the smoke absorption liquid that obtains containing Sulfothiorine and S-WAT;
And step 7, the smoke absorption liquid in the step 6 is added in the retort, add sulphur, temperature reaction is filtered then, is concentrated, filtration, crystallization, centrifugal classification promptly get the Sulfothiorine finished product.
Wherein, described converter is the structure of box hat inner lining refractory, drives converter with machinery and rotates around axis, and converter is spindle-type, and is small at both ends and big in the middle, and burner is equipped with heating unit, and the stove tail communicates with secondary combustion chamber or flue; Concentrated residue to be burned can add the bosh from burner or stove tail; Bosh has discharge port; Be used to emit the slag after the burning.
First embodiment
See also Fig. 1, first embodiment of the invention realizes as follows:
Step 1, material concentrates: produce with sodium formate method and obtain distillation residual liquid 111 after methyl alcohol is reclaimed in the mother liquor rectifying that produces in the V-Brite B process, described distillation residual liquid 111 main component content are that sodium formiate 110g/l, S-WAT 8.9g/l, Sulfothiorine 4.5g/l, methyl alcohol 6.5g/l, organic sulfide and other material 61g/l, chemical oxygen demand (COD) are 238000mg/l, get 10m
3Above-mentioned distillation residual liquid 111 is concentrated into and a large amount of crystal occur, emits the concentrated residue 112 that obtains being the pulp thing after the cooling, and weight is 2020kg;
Step 2, burn the charging stage: burn with two sections converters 121, adopt heavy oil burner earlier temperature in the converter to be risen to 1080 ℃, concentrated residue 112 personnel selection of step 1 had a rest break add in the primary zone of converter 112, bubbling air is also regulated air capacity, concentrated residue 112 is burnt in the primary zone of converter obtain incineration residue 122 and tail gas, tail gas burns to produce in the secondary combustion chamber of converter 121 and contains SO
2 Incineration flue gas 123, this moment converter 121 secondary combustion chambers stove in temperature be 1250 ℃, when the indoor incineration residue 122 of converter 121 primary combustions reach furnace volume 1/5 the time, stop into concentrated residue 112;
Step 3, the fusion blowing: keeping converter 121 interior temperature is 1100 ℃, makes incineration residue 122 basic fusions, opens the drain hole of converter 121, and the burning slag 122 that will be molten state is poured out;
Step 4, blowing finishes, and closes drain hole, enters the operation of step 2 once more;
Step 5, the incineration residue 122 that analytical procedure 3 obtains, its main component is a yellow soda ash 70%, sodium oxide 8.2%, sodium sulphite 8.1%; Will be wherein a part of incineration residue 122 water dissolution, filter out insolubles after, obtain incineration residue lysate 151 to use for step 6; Another part incineration residue 122 offers other industry and uses through cooling, broken, packing;
Step 6, smoke absorption: SO2 content is 15800mg/m in the incineration flue gas 123 that produces in the step 2
3To send in the one-level tail gas washing tower 161 after incineration flue gas 123 coolings, with pump 162 the incineration residue lysate 151 that obtains in an amount of step 5 is added in the one-level tail gas washing tower 161, and spray is inhaled the SO2 in the incineration flue gas 123, incineration flue gas 123 is sent into secondary tail gas washing tower 163 and is added NaOH to secondary tail gas washing tower 163, make incineration flue gas 123 obtain smoke absorption liquid 164 after secondary tail gas washing tower 163 washing and with the flue tail gas discharging, analyzing the content of sulfur dioxide that secondary tail gas washing tower 163 discharges flue gases is 390mg/m
3, flue gas does not have stink, and the main component of analyzing smoke absorption liquid 164 is Sulfothiorine 35g/l, S-WAT 175g/l;
Step 7, add reaction of Salmon-Saxl system Sulfothiorine, smoke absorption liquid in the step 6 164 is added in the reaction of Salmon-Saxl jar 171, add a certain amount of sulphur, temperature reaction, again through filtration 172, concentrate 173, insulation filters 174, promptly to get content be 98.2% five water Sulfothiorine 177 (hypo finished product) 3200kg for crystallization 175, centrifugal classification 176.
Second embodiment
See also Fig. 2, second embodiment of the invention realizes as follows:
Step 1, material concentrates: produce with sodium formate method and obtain distillation residual liquid 211 after methyl alcohol is reclaimed in the mother liquor rectifying that produces in the V-Brite B process, described distillation residual liquid 211 main component content are that sodium formiate 120g/l, S-WAT 7.8g/l, Sulfothiorine 5.6g/l, methyl alcohol 5.8g/l, organic sulfide and other material 63g/l, chemical oxygen demand (COD) are 252000mg/l, get 10m
3Above-mentioned distillation residual liquid 211 is concentrated into a large amount of crystal of appearance and becomes concentrated raffinate 213, to add that methyl alcohol filter out with sodium formiate and S-WAT be that the crystal 2 14 of main component obtains methyl alcohol leaching filtrate 215 to concentrating raffinate 213, crystal 2 14 weight are 1120kg, its main component sodium formiate content is 87%, S-WAT 7.1g/l, is used for the synthetic of V-Brite B; Evaporation contains the methyl alcohol leaching filtrate 215 recovery methyl alcohol of methyl alcohol then, residuum is the concentrated residue that is in a liquid state 212 of good fluidity, weight is 980kg, evaporation contains the filtrate of methyl alcohol and reclaims methyl alcohol, the remaining concentrated residue good fluidity in methyl alcohol evaporation back, be convenient to carry and metering, be used for burning and be easy to realize mechanize;
Step 2, burn the charging stage: combination 221 devices with converter and stationary furnace burn, adopt heavy oil burner earlier temperature in the converter to be risen to 1120 ℃, in of the concentrated residue 212 continuous suction converters of first pump 224 with liquid state, bubbling air is also regulated air capacity, concentrated residue 212 is burnt in converter obtains incineration residue 222 and tail gas, tail gas again in stationary furnace secondary combustion obtain containing SO
2 Incineration flue gas 223, during secondary combustion in the stationary furnace stove temperature be 1180 ℃, when the incineration residue in the converter 222 reach furnace volume 1/4 the time, stop into concentrated residue 212;
Step 3, the fusion blowing: keeping the interior temperature of converter is 1100 ℃, when incineration residue 222 basic fusions, opens the drain hole of converter, and the incineration residue 222 of molten state is poured out;
Step 4, blowing finishes, and closes drain hole, enters the operation of step 2 once more;
Step 5, slag is burned in dissolving: the incineration residue 222 that analytical procedure 3 obtains, main component are yellow soda ash 48%, sodium oxide 12%, sodium sulphite 28%; Water is dissolved in the incineration residue 222 that obtains in the step 3, filters out insolubles then and obtains burning slag lysate 251;
Step 6, smoke absorption: SO in the incineration flue gas 223 that produces in the step 2
2Content is 48800mg/m
3, incineration flue gas 223 is sent in the one-level tail gas washing tower 261, with second pump 262 the incineration residue lysate 251 that obtains in an amount of step 5 is added in the one-level tail gas washing tower 261, spray absorbs the SO in the incineration flue gas 223
2 Incineration flue gas 223 is sent into secondary tail gas washing tower 263 and is added NaOH to secondary tail gas washing tower 263, incineration flue gas 2232 obtains smoke absorption liquid 264 and with the flue tail gas discharging, analyzes the SO in the flue gas of discharging tail gas washing tower after 263 washings of secondary tail gas washing tower
2Content is 312mg/m
3, flue gas does not have stink, and the main component of analyzing smoke absorption liquid 264 is Sulfothiorine 63g/l and S-WAT 135g/l;
Step 7, add reaction of Salmon-Saxl system Sulfothiorine: the smoke absorption liquid in the step 6 264 is added in the reaction of Salmon-Saxl jar 271, add a certain amount of sulphur, temperature reaction, again through filtration 272, concentrate 273, insulation filters 274, promptly to get content be 99.2% five water Sulfothiorine 277 (hypo) 1250kg for crystallization 275, centrifugal classification 276.
Claims (7)
1. the treatment process that sodium formate method is produced the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process is characterized in that, comprises the steps:
Step 1 is produced in the V-Brite B process at sodium formate method, the raffinate behind the mother liquor rectifying recovery methyl alcohol is concentrated obtain concentrated residue or the raffinate behind the mother liquor rectifying recovery methyl alcohol is obtained concentrated residue after concentrating the recovery sodium formiate;
Step 2, in the combination stove of a section or two sections converters or converter and stationary furnace, adopt liquid or gas fuel combustion, when furnace temperature is raised to 600-1300 ℃, concentrated residue is sent in the converter continuously or intermittently, regulate the air capacity that feeds simultaneously, the burning concentrated residue obtains containing the incineration flue gas of sulfurous gas, keeps furnace temperature in the combustion processes at 600-1300 ℃;
Step 3 stops concentrated residue being sent in the converter, keeps temperature in the converter, makes and burns the slag fusion, opens the drain hole of converter, and the burning slag of molten state is poured out;
Step 4, blowing finishes, and closes drain hole, enters the operation of step 2 once more;
Step 5 will be burned slag and will be dissolved into the aqueous solution, filter out insolubles then;
Step 6, the incineration flue gas that burning concentrated residue in the step 2 obtains is sent in the tail gas washing tower, add the aqueous solution that obtains in an amount of step 5 in tail gas washing tower, the sulfurous gas in the incineration flue gas is absorbed the smoke absorption liquid that obtains containing Sulfothiorine and S-WAT; And
Step 7 adds the smoke absorption liquid in the step 6 in the retort, adds sulphur, and temperature reaction is filtered, concentrates, is incubated filtration, crystallization, centrifugal classification then and promptly gets five water Sulfothiorine finished products.
2. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, it is characterized in that: in the step 1, after distillation residual liquid concentrated, when the recovery sodium formiate is the crystal of main component, add methyl alcohol leaching, washing crystal, filter then, the crystal that leaches is used for the synthetic of V-Brite B.
3. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, it is characterized in that: described converter is the structure of box hat inner lining refractory, driving converter with machinery rotates around axis, converter is spindle-type, two is little, broad in the middle, burner is equipped with heating unit, and the stove tail communicates with secondary combustion chamber or flue; Concentrated residue to be burned can add the bosh from burner or stove tail; Bosh has discharge port; Be used to emit the slag after the burning.
4. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, it is characterized in that: in step 3, when material in the converter reaches the 1/8-1/2 of furnace volume, stop into concentrated residue.
5. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, it is characterized in that: in step 3, keep the interior temperature of converter to be higher than the slag fusing point, temperature is 750～900 ℃ in the converter.
6. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, it is characterized in that: in step 6, incineration flue gas is sent into earlier in the one-level tail gas washing tower, in the one-level tail gas washing tower, add the incineration residue lysate in the step 5, spray absorbs sulfur in smoke, and incineration flue gas is discharging after the washing of secondary tail gas washing tower again.
7. a kind of sodium formate method according to claim 1 is produced the treatment process of the raffinate behind the mother liquor rectifying recovery methyl alcohol in the V-Brite B process, and it is characterized in that: the slag that obtains in step 3 is as the alkaline sodium salt byproduct.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200710027443XA CN101081715B (en) | 2007-04-06 | 2007-04-06 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200710027443XA CN101081715B (en) | 2007-04-06 | 2007-04-06 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
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| CN101081715A CN101081715A (en) | 2007-12-05 |
| CN101081715B true CN101081715B (en) | 2010-07-28 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570267B (en) * | 2013-08-19 | 2016-04-06 | 广东中成化工股份有限公司 | The method of grinding aid is manufactured with V-Brite B residue |
| CN103641077B (en) * | 2013-12-16 | 2015-12-09 | 浙江嘉成化工有限公司 | A kind of circulation utilization method of sodium hydrosulfite wastewater |
| CN103755048A (en) * | 2013-12-30 | 2014-04-30 | 中盐安徽红四方股份有限公司 | New sodium hydrosulfite wastewater treatment method |
| CN104177248B (en) * | 2014-08-25 | 2015-09-09 | 湖南中成化工有限公司 | A kind of distillation residual liquid treatment process of vat powder mother liquor |
| CN105016312B (en) * | 2015-07-08 | 2017-03-01 | 湖南龙盛环保有限公司 | A kind of method that in sodium hydrosulfite production, sulfur containing waste material recycles |
| CN105585192B (en) * | 2015-12-25 | 2018-03-09 | 石家庄杰克化工有限公司 | A kind of method of wastewater treatment of 4,6 dihydroxy-pyrimidine production |
| CN106706841B (en) * | 2016-12-13 | 2019-02-05 | 柳州化工股份有限公司 | The analysis method of sodium formate purity is recycled in sodium hydrosulfite production |
| CN109053422A (en) * | 2018-09-21 | 2018-12-21 | 浙江嘉成化工有限公司 | The processing method and equipment of insurance powder waste liquid in sodium hydrosulfite production process |
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