CN102512931B - Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production - Google Patents
Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production Download PDFInfo
- Publication number
- CN102512931B CN102512931B CN201110406243.1A CN201110406243A CN102512931B CN 102512931 B CN102512931 B CN 102512931B CN 201110406243 A CN201110406243 A CN 201110406243A CN 102512931 B CN102512931 B CN 102512931B
- Authority
- CN
- China
- Prior art keywords
- solution
- tail gas
- acyl chlorides
- reactor
- feed liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 150000001263 acyl chlorides Chemical class 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 title abstract 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000010521 absorption reaction Methods 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical class [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 17
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 50
- 239000007788 liquid Substances 0.000 claims description 34
- 230000009102 absorption Effects 0.000 claims description 30
- 239000011734 sodium Substances 0.000 claims description 23
- 229940001482 sodium sulfite Drugs 0.000 claims description 22
- 235000010265 sodium sulphite Nutrition 0.000 claims description 22
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 10
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012047 saturated solution Substances 0.000 claims description 5
- 239000013589 supplement Substances 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 230000009469 supplementation Effects 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 abstract description 8
- 239000012527 feed solution Substances 0.000 abstract 4
- 238000007599 discharging Methods 0.000 abstract 2
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 19
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 11
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 238000010923 batch production Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 description 1
- 235000010261 calcium sulphite Nutrition 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Landscapes
- Treating Waste Gases (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention relates to a method for preparing sodium hydrosulphite by the utilization of tail gas from acyl chloride production. The method has advantages of high absorptivity of sulfur dioxide, high absorption efficiency of sulfur dioxide, good sodium hydrosulphite product quality and product quality stability. The method comprises the following steps of: (1) absorbing the tail gas from acyl chloride production through water and removing HCl gas; (2) removing a few HCl gas from sulfur dioxide by the use of a saturated sodium bisulfite solution; (3) allowing the acyl chloride production tail gas processed from the step (2) to enter into a continuous feeding and continuous discharging absorption kettle filled with a sodium carbonate solution, carrying out three-stage continuous absorption of sulfur dioxide at normal pressure at 40-110 DEG C to generate a sodium bisulfite containing feed solution, discharging the feed solution, and controlling pH of the discharged feed solution within 3.9-5.9; and (4) neutralizing the discharged feed solution from the step (3) by the use of alkali until pH is within 8.0-10.0 to obtain a neutralizer, wherein the alkali is a NaOH solution or a Na2CO3 solution.
Description
Technical field
The present invention relates to a kind of preparation method of sodium sulfite, particularly relate to a kind of acyl chlorides that utilizes and produce the method that tail gas is prepared sodium sulfite.
Background technology
While utilizing thionyl chloride method to produce acyl chlorides, the processing problem of hydrogen chloride in tail gas and sulfur dioxide is the difficult problem of the sector always.Along with continuous expansion and the fast development of China's acyl chlorides industry production scale, as acyl chlorides, produce the main component of tail gas, the processing of hydrogen chloride is relatively easy, and the processing of sulfur dioxide is comparatively difficult.At present, the processing of acyl chlorides production hydrogen chloride in tail gas mainly adopts water absorption method, and the processing method of sulfur dioxide mainly contains: adopt alkali lye to carry out batch process absorption and absorb two kinds of methods with lime.Adopt alkali lye carry out batch process absorb refer to adopt batch process, the SO 2 tail gas in acyl chlorides being produced with alkali lye or soda ash solution absorbs, neutralize, concentrated and be dried to prepare the method for sodium sulfite; Lime absorption process refers to the method that direct employing limewash absorbs SO 2 tail gas.Former approach has the shortcomings such as sulfur dioxide absorption efficiency is not high, unstable product quality; It is a kind of relatively backward method that lime absorbs, and its absorption rate of sulfur dioxide is not high, and the calcium sulfite use of generation is also little.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of absorption rate of sulfur dioxide is high, sulfur dioxide absorption efficiency is high, the acyl chlorides that utilizes of sodium sulfite good product quality and constant product quality is produced the method that tail gas is prepared sodium sulfite.
Utilize acyl chlorides to produce the method that tail gas is prepared sodium sulfite, comprise the following steps:
(1) acyl chlorides is produced tail gas through water absorption, removes HCl gas wherein; Can obtain the concentrated hydrochloric acid that mass fraction is 28-32%;
(2) with saturated solution of sodium bisulfite, remove a small amount of HCl gas being mixed with in sulfur dioxide;
(3) step (2) was processed acyl chlorides is produced tail gas and is passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor under the condition of normal pressure, 40-110 ℃ and carry out three grades of continuous sulfur dioxide absorptions, generate and contain the feed liquid of sodium hydrogensulfite and emit, the pH that feed liquid is emitted in control is 3.9-5.9; Wherein: three grades of continuous absorption equipment therefors comprise the first reactor, the second reactor, the 3rd reactor, the first to the 3rd reactor is connected in turn by pipeline, and Na is all housed in each reactor
2cO
3solution, the acyl chlorides that step (2) was processed is produced tail gas and is passed into the first reactor and Na
2cO
3solution reaction, the SO that the first reactor fails to sponge
2, by pipeline, enter second and third reactor and again absorb.Na in reactor
2cO
3solution and SO
2reaction, generates containing NaHSO
3feed liquid, during work, in the first reactor, emit continuously containing NaHSO
3feed liquid, first reactor reduce feed liquid adopt press over system by the second reactor supplement Na
2cO
3solution, the second reactor supplements Na by the 3rd reactor
2cO
3solution, by the Na preparing
2cO
3solution continuous supplementation is in the 3rd reactor; During three grades of continuous absorptions, the Na between first, second and third reactor
2cO
3solution flow rate size is relevant with the pH size containing the feed liquid of sodium hydrogensulfite in the first reactor, by automatic regulating valve, controlled, when the pH that contains the pH of sodium hydrogensulfite feed liquid in the first reactor and emit feed liquid control differs larger, and the Na between reactor
2cO
3solution flow rate is large; When differing hour containing the pH of sodium hydrogensulfite feed liquid and the pH that emits feed liquid control in the first reactor, the Na between reactor
2cO
3solution flow rate is little.Reaction equation is as follows:
Na
2CO
3+2SO
2+H
2O＝2NaHSO
3+CO
2；
(4) the feed liquid alkali that step (3) is emitted neutralizes, and to pH value, for 8.0-10.0 stops, obtains neutralizer, and wherein said alkali is NaOH solution or Na
2cO
3solution.Sodium hydrogensulfite and alkali reaction generate sodium sulfite.Reaction equation is:
Na
2CO
3+2NaHSO
3＝2Na
2SO
3+CO
2+H
2O；
The present invention utilizes acyl chlorides to produce the method that tail gas is prepared sodium sulfite, wherein said step (3) is: the acyl chlorides that step (2) was processed is produced tail gas and passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor, under normal pressure, the condition of 70 ℃, carry out three grades of continuous sulfur dioxide absorptions, generate and contain the feed liquid of sodium hydrogensulfite and emit, the pH that feed liquid is emitted in control is 4.9;
The present invention utilizes acyl chlorides to produce tail gas to prepare the method for sodium sulfite, also comprises that neutralizer obtains anhydrous sodium sulfite through evaporative crystallization, after centrifugal, dry after wherein said step (4).
The present invention utilizes acyl chlorides to produce the method that tail gas is prepared sodium sulfite, wherein NaOH solution or Na described in step (4)
2cO
3the mass fraction of solution is 30-35%.
The present invention utilizes acyl chlorides to produce the method that tail gas is prepared sodium sulfite, wherein Na described in step (3)
2cO
3the concentration of solution is 200g/L-250g/L.
The present invention utilizes acyl chlorides to produce the method that tail gas is prepared sodium sulfite, and wherein said acyl chlorides is produced tail gas and absorbed and adopt three grades of falling liquid film water absorption methods through water.
The present invention utilizes acyl chlorides to produce method that tail gas prepares sodium sulfite compared with prior art, and its absorption rate of sulfur dioxide reaches more than 99.8%; Compared with producing sodium sulfite with original employing batch process, the output of sodium sulfite is brought up to 11.2 tons by producing 8.3 tons original every day, has improved 35%, and the treating capacity of acyl chlorides being produced to tail gas has also improved 30-40%; And product sodium sulfite purity reaches country-level standard; Compared with batch process, the operate miss between continuous absorption does not have batch, product quality is more stable.
Below in conjunction with accompanying drawing, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes acyl chlorides to produce the flow chart that tail gas is prepared the method for anhydrous sodium sulfite;
The specific embodiment
Embodiment 1
(1) acyl chlorides is produced tail gas through the absorption of falling liquid film water, removes HCl gas wherein, the concentrated hydrochloric acid that generation mass fraction is 30%;
(2) with saturated solution of sodium bisulfite, remove a small amount of HCl gas being mixed with in sulfur dioxide;
(3) acyl chlorides that step (2) was processed is produced tail gas and is passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor that concentration is 200g/L, under normal pressure, the condition of 40 ℃, carry out three grades of continuous sulfur dioxide absorptions, generate and contain the feed liquid of sodium hydrogensulfite and emit, the pH that feed liquid is emitted in control is 5.9;
(4) the NaOH solution that the feed liquid mass fraction that step (3) is emitted is 30% neutralizes, to pH value be 10.0 only, obtain neutralizer.
Absorptivity by above-mentioned steps sulfur dioxide reaches more than 99.8%, then by neutralizer carry out condensing crystallizing, centrifugal and dry after obtain anhydrous sodium sulfite, product reaches country-level standard.
Embodiment 2
(1) acyl chlorides is produced tail gas through the absorption of falling liquid film water, removes HCl gas wherein, the concentrated hydrochloric acid that generation mass fraction is 32%;
(2) with saturated solution of sodium bisulfite, remove a small amount of HCl gas being mixed with in sulfur dioxide;
(3) acyl chlorides that step (2) was processed is produced tail gas and is passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor that concentration is 250g/L, under normal pressure, the condition of 110 ℃, carry out three grades of continuous sulfur dioxide absorptions, generate and contain the feed liquid of sodium hydrogensulfite and emit, the pH that feed liquid is emitted in control is 3.9;
(4) Na that the feed liquid mass fraction that step (3) is emitted is 30%
2cO
3solution neutralizes, to pH value be 8.0 only, obtain neutralizer.
Absorptivity by above-mentioned steps sulfur dioxide reaches more than 99.8%, then by neutralizer carry out condensing crystallizing, centrifugal and dry after obtain anhydrous sodium sulfite, product reaches country-level standard.
Embodiment 3
(1) acyl chlorides is produced tail gas through the absorption of falling liquid film water, removes HCl gas wherein, the concentrated hydrochloric acid that generation mass fraction is 28%;
(2) with saturated solution of sodium bisulfite, remove a small amount of HCl gas being mixed with in sulfur dioxide;
(3) acyl chlorides that step (2) was processed is produced tail gas and is passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor that concentration is 225g/L, under normal pressure, the condition of 70 ℃, carry out three grades of continuous sulfur dioxide absorptions, generate and contain the feed liquid of sodium hydrogensulfite and emit, the pH that feed liquid is emitted in control is 4.9;
(4) Na that the feed liquid mass fraction that step (3) is emitted is 35%
2cO
3solution neutralizes, to pH value be 9.0 only, obtain neutralizer.
Absorptivity by above-mentioned steps sulfur dioxide reaches more than 99.8%, then by neutralizer carry out condensing crystallizing, centrifugal and dry after obtain anhydrous sodium sulfite, product reaches country-level standard.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (5)
1. utilize acyl chlorides to produce the method that tail gas is prepared sodium sulfite, it is characterized in that comprising the following steps:
(1) acyl chlorides is produced tail gas through water absorption, removes HCl gas wherein;
(2) with saturated solution of sodium bisulfite, remove a small amount of HCl gas being mixed with in sulfur dioxide;
(3) acyl chlorides that step (2) was processed is produced tail gas and is passed into continuous feed and continuous discharge and be equipped with in the absorption kettle of sodium carbonate liquor, under the condition of 110 ℃ of normal pressures, 40 ?, carry out three grades of continuous sulfur dioxide absorptions, generate containing the feed liquid of sodium hydrogensulfite and emit this feed liquid, control the pH value of emitting feed liquid and be 3.9 ?5.9;
(4) the feed liquid alkali that step (3) is emitted neutralizes, to pH value be 8.0 ?10.0 only, obtain neutralizer, wherein said alkali is NaOH solution or Na
2cO
3solution;
Wherein, in step (3), Na in reactor
2cO
3solution and SO
2reaction, generates containing NaHSO
3feed liquid, during work, in the first reactor, emit continuously containing NaHSO
3feed liquid, first reactor reduce feed liquid adopt press over system by the second reactor supplement Na
2cO
3solution, the second reactor supplements Na by the 3rd reactor
2cO
3solution, by the Na preparing
2cO
3solution continuous supplementation is in the 3rd reactor.
2. according to claim 1ly utilize acyl chlorides to produce tail gas to prepare the method for sodium sulfite, it is characterized in that: after described step (4), also comprise that neutralizer obtains anhydrous sodium sulfite through evaporative crystallization, after centrifugal, dry.
3. the acyl chlorides that utilizes according to claim 2 is produced the method that tail gas is prepared sodium sulfite, it is characterized in that: described NaOH solution or Na
2cO
3the mass fraction of solution be 30 ?35%.
4. the acyl chlorides that utilizes according to claim 3 is produced the method that tail gas is prepared sodium sulfite, it is characterized in that: described Na
2cO
3the concentration of solution be 200g/L ?250g/L.
5. the acyl chlorides that utilizes according to claim 4 is produced the method that tail gas is prepared sodium sulfite, it is characterized in that: described acyl chlorides is produced tail gas and absorbed and adopt three grades of falling liquid film water absorption methods through water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110406243.1A CN102512931B (en) | 2011-12-08 | 2011-12-08 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110406243.1A CN102512931B (en) | 2011-12-08 | 2011-12-08 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
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| Publication Number | Publication Date |
|---|---|
| CN102512931A CN102512931A (en) | 2012-06-27 |
| CN102512931B true CN102512931B (en) | 2014-04-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109289481A (en) * | 2018-10-25 | 2019-02-01 | 老河口市天和科技有限公司 | Sulfonic chloride produces gas recovery system and technique |
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| CN102824820A (en) * | 2012-08-27 | 2012-12-19 | 安徽常泰化工有限公司 | Treatment technology for tail gas generated from production process of cis-Z-3-(2-chloro-3, 3, 3-triflulo-1-propenyl)-2, 2-dimethyl cyclopropane carbonyl chloride |
| CN102976946A (en) * | 2012-12-13 | 2013-03-20 | 烟台泰和新材料股份有限公司 | Method for synthesizing dimethyl isophthalate |
| CN102989265A (en) * | 2012-12-13 | 2013-03-27 | 烟台泰和新材料股份有限公司 | Treatment method of acyl chloride production tail gas |
| CN103332751B (en) * | 2013-05-22 | 2015-08-26 | 玉门市翔宇环保有限公司 | Ferrous sulfate method of comprehensive utilization |
| CN104587822A (en) * | 2015-01-22 | 2015-05-06 | 贵州兰鑫石墨机电设备制造有限公司 | Separation device for hydrogen chloride and sulfur dioxide as well as separation method thereof |
| CN109455742B (en) * | 2019-01-06 | 2021-01-12 | 曲阜师范大学 | Method for simply producing pharmaceutic adjuvant anhydrous sodium sulfite |
| CN112939028B (en) * | 2020-11-03 | 2023-05-26 | 宣城市楷昂化工有限公司 | Preparation method of sodium sulfite |
| CN113003587A (en) * | 2021-03-02 | 2021-06-22 | 安徽金轩科技有限公司 | Continuous production method for recovering sodium sulfite from thionyl chloride tail gas |
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| CN101342441A (en) * | 2008-08-20 | 2009-01-14 | 江苏扬农化工股份有限公司 | Method for treating tail gas of acyl chlorination |
| CN101412526A (en) * | 2008-01-18 | 2009-04-22 | 江西世龙实业股份有限公司 | Method for preparing sodium sulphite with tail gas from thionyl chloride synthesis process |
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2011
- 2011-12-08 CN CN201110406243.1A patent/CN102512931B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412526A (en) * | 2008-01-18 | 2009-04-22 | 江西世龙实业股份有限公司 | Method for preparing sodium sulphite with tail gas from thionyl chloride synthesis process |
| CN101343038A (en) * | 2008-06-30 | 2009-01-14 | 常熟富士莱医药化工有限公司 | Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation |
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Address after: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Patentee after: Taihe New Material Group Co.,Ltd. Patentee after: YANTAI YUXIANG FINE CHEMICAL Co.,Ltd. Address before: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Patentee before: YANTAI TAYHO ADVANCED MATERIALS Co.,Ltd. Patentee before: YANTAI YUXIANG FINE CHEMICAL Co.,Ltd. |
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Effective date of registration: 20231213 Address after: 750411 Ningxia Ningdong Energy and Chemical Base Coal Chemical Industry Park, Yinchuan City, Ningxia Hui Autonomous Region, north of Yinglite Project Park Road and east of parking lot Patentee after: Ningxia Ningdong Taihe Chemical Technology Co.,Ltd. Patentee after: Taihe New Material Group Co.,Ltd. Address before: 264006 No. 10, Heilongjiang Road, Yantai economic and Technological Development Zone, Yantai, Shandong Patentee before: Taihe New Material Group Co.,Ltd. Patentee before: YANTAI YUXIANG FINE CHEMICAL Co.,Ltd. |