CN109455742B - A kind of method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient - Google Patents
A kind of method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient Download PDFInfo
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- CN109455742B CN109455742B CN201910010047.9A CN201910010047A CN109455742B CN 109455742 B CN109455742 B CN 109455742B CN 201910010047 A CN201910010047 A CN 201910010047A CN 109455742 B CN109455742 B CN 109455742B
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- sodium sulfite
- anhydrous sodium
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- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 title claims abstract description 68
- 229940101006 anhydrous sodium sulfite Drugs 0.000 title claims abstract description 49
- 239000000546 pharmaceutical excipient Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 40
- 229940124531 pharmaceutical excipient Drugs 0.000 title claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 claims abstract description 29
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 22
- 239000012535 impurity Substances 0.000 claims description 16
- 238000001514 detection method Methods 0.000 claims description 12
- 238000001704 evaporation Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 229940001482 sodium sulfite Drugs 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 6
- 238000007738 vacuum evaporation Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 235000013373 food additive Nutrition 0.000 claims description 3
- 239000002778 food additive Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 claims description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000005292 vacuum distillation Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910001948 sodium oxide Inorganic materials 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 238000000926 separation method Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种简易生产药用辅料无水亚硫酸钠的方法,涉及化工领域,工艺步骤包括:利用蒸馏水配置一定浓度的亚硫酸氢钠溶液,在一定反应温度下,边搅拌边加入一定浓度氢氧化钠溶液,控制反应终点的pH值为碱性,搅拌反应20min左右;反应结束后,继续搅拌控制反应终点的pH值在12.0~12.30范围内;将反应液进行减压真空蒸馏,蒸发至反应液出现大量结晶,然后冷却,离心分离,固体结晶经干燥,所得产品进行分析检测,合格即为药用辅料无水亚硫酸钠。本发明利用食品级的亚硫酸氢钠与精制氢氧化钠为原料,经一步反应制取医药辅料无水亚硫酸钠的生产方法,具有工艺流程短、操作简便的特点,而且经过原料、生产环节及产品的检测,确保产品质量。
The invention discloses a method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient, and relates to the field of chemical industry. The process steps include: using distilled water to prepare a sodium bisulfite solution of a certain concentration, and adding a certain concentration of hydrogen while stirring at a certain reaction temperature Sodium oxide solution, control the pH value of the reaction end point to be alkaline, and stir the reaction for about 20min; after the reaction is completed, continue to stir to control the pH value of the reaction end point to be in the range of 12.0 to 12.30; the reaction solution is subjected to reduced pressure vacuum distillation and evaporated to the reaction A large amount of crystals appeared in the liquid, then cooled, centrifuged, and the solid crystals were dried. The obtained product was analyzed and tested, and it was qualified as anhydrous sodium sulfite as a pharmaceutical excipient. The present invention utilizes food-grade sodium bisulfite and refined sodium hydroxide as raw materials, and a production method for preparing anhydrous sodium sulfite as a pharmaceutical auxiliary material through one-step reaction has the characteristics of short technological process and simple and convenient operation. Product testing to ensure product quality.
Description
Name of material | Index (I) |
Concentration of sodium bisulfite solution, kg/m3 | 260 |
Concentration of sodium hydroxide solution, kg/m3 | 60 |
Amount of sodium bisulfite solution added, m3 | 0.6 |
Reaction temperature of | 43 |
Reaction end point pH value | 12.10 |
Vacuum degree of vacuum evaporation and concentration | 35kPa |
Amount of mother liquor after separation of crystals, m3 | 0.2 |
Drying temperature of | 230 |
Theoretical yield of anhydrous sodium sulfite, kg | 188.95 |
Actual yield of anhydrous sodium sulfite kg | 156.0 |
Yield of anhydrous sodium sulfite% | 82.56 |
Anhydrous sodium sulfite product detection | Qualified |
Claims (5)
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CN201910010047.9A CN109455742B (en) | 2019-01-06 | 2019-01-06 | A kind of method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient |
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CN201910010047.9A CN109455742B (en) | 2019-01-06 | 2019-01-06 | A kind of method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient |
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CN109455742A CN109455742A (en) | 2019-03-12 |
CN109455742B true CN109455742B (en) | 2021-01-12 |
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CN201910010047.9A Active CN109455742B (en) | 2019-01-06 | 2019-01-06 | A kind of method for simply producing anhydrous sodium sulfite as a pharmaceutical excipient |
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Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111439759A (en) * | 2020-05-23 | 2020-07-24 | 淄博长城化工厂 | Method for producing food-grade potassium sulfite by adopting potassium metabisulfite mother liquor |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02199017A (en) * | 1989-01-30 | 1990-08-07 | Sumitomo Metal Mining Co Ltd | Production of sodium sulfite |
CN1762809A (en) * | 2005-09-02 | 2006-04-26 | 吕国锋 | Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate |
CN102512931A (en) * | 2011-12-08 | 2012-06-27 | 烟台泰和新材料股份有限公司 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
CN102887533A (en) * | 2012-09-28 | 2013-01-23 | 天津中科化工有限公司 | Method for producing anhydrous Na2SO3 by using alkali-containing waste mother liquor |
CN103570046A (en) * | 2013-11-14 | 2014-02-12 | 湖南恒光化工有限公司 | Process for preparing high-purity sodium sulfite through sulfuric acid production industrial exhaust |
CN103880043A (en) * | 2012-12-23 | 2014-06-25 | 吕子玉 | Sodium hydrosulfite production method |
CN106943859A (en) * | 2016-01-07 | 2017-07-14 | 刘炳福 | One kind administers S0 in flue gas2The method for producing anhydrous sodium sulfite |
-
2019
- 2019-01-06 CN CN201910010047.9A patent/CN109455742B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02199017A (en) * | 1989-01-30 | 1990-08-07 | Sumitomo Metal Mining Co Ltd | Production of sodium sulfite |
CN1762809A (en) * | 2005-09-02 | 2006-04-26 | 吕国锋 | Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate |
CN102512931A (en) * | 2011-12-08 | 2012-06-27 | 烟台泰和新材料股份有限公司 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
CN102887533A (en) * | 2012-09-28 | 2013-01-23 | 天津中科化工有限公司 | Method for producing anhydrous Na2SO3 by using alkali-containing waste mother liquor |
CN103880043A (en) * | 2012-12-23 | 2014-06-25 | 吕子玉 | Sodium hydrosulfite production method |
CN103570046A (en) * | 2013-11-14 | 2014-02-12 | 湖南恒光化工有限公司 | Process for preparing high-purity sodium sulfite through sulfuric acid production industrial exhaust |
CN106943859A (en) * | 2016-01-07 | 2017-07-14 | 刘炳福 | One kind administers S0 in flue gas2The method for producing anhydrous sodium sulfite |
Non-Patent Citations (1)
Title |
---|
高纯无水亚硫酸钠生产工艺研究;耿斌 等;《无机盐工业》;20140331;第46卷(第3期);54-56 * |
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Effective date of registration: 20211112 Address after: 257000 room b420, No. 59, Fuqian street, Dongying District, Dongying City, Shandong Province Patentee after: Dongying Guangli Lingang Industrial Park Co.,Ltd. Address before: 273165 No. 57, Jingxuan West Road, Qufu City, Jining City, Shandong Province Patentee before: QUFU NORMAL University |
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Effective date of registration: 20221226 Address after: 257000 room b420, No. 59, Fuqian street, Dongying District, Dongying City, Shandong Province Patentee after: Dongying Guangli Lingang Industrial Park Co.,Ltd. Patentee after: Dongying Guangli Port Park Operation Co.,Ltd. Address before: 257000 room b420, No. 59, Fuqian street, Dongying District, Dongying City, Shandong Province Patentee before: Dongying Guangli Lingang Industrial Park Co.,Ltd. |