CN102250093B - Process for recovering theophylline sodium salt from theophylline sodium salt mother liquid - Google Patents
Process for recovering theophylline sodium salt from theophylline sodium salt mother liquid Download PDFInfo
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- CN102250093B CN102250093B CN 201110160619 CN201110160619A CN102250093B CN 102250093 B CN102250093 B CN 102250093B CN 201110160619 CN201110160619 CN 201110160619 CN 201110160619 A CN201110160619 A CN 201110160619A CN 102250093 B CN102250093 B CN 102250093B
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- theophylline sodium
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- theophylline
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Abstract
The invention relates to a recovery process of a theophylline sodium salt. The process is characterized by comprising the following steps: neutralizing a theophylline sodium salt mother liquid with an acid liquid, absorbing a neutralization liquid through an absorption tower and then carrying out resolution, wherein 50-60% by weight of dilute sulphuric acid is used as the acid liquid, the pH of the acid liquid is 4.5-6, and a macroporous adsorption resin is used as an adsorbent in the absorption tower. The process has the advantages that (1) an organic solvent is not used, and chemical oxygen demand (COD) and ammonia nitrogen content are not increased; (2) operation cost is low; (3) energy consumption is low; (4) the recovery rate of the theophylline sodium salt is improved; (5) operation is simple, labor intensity is reduced, work environment is improved, and a safety factor is improved; and (6) whole optimization is carried out by combining former and latter processes, thereby achieving the purpose of environmentally-friendly production.
Description
Technical field
The invention belongs to field of medicine and chemical technology, particularly the mother liquid recovery process in a kind of caffeine intermediate preparation process.
Background technology
The theophylline sodium salt is called for short tea sodium; important intermediate for caffeine production; manufacturer all adopts traditional processing technology both at home and abroad: use Mono Chloro Acetic Acid to be starting raw material; through neutralization-cyaniding-acidifying-condensation-cyclization-nitrosification-reduction-acidylate-closed loop-centrifugation; obtain solid tea sodium and be applied to lower operation (first chemical industry order); contain 0.5%-0.7% tea sodium in the centrifuge mother liquor, the tea sodium content is 600t/y in the plant mother liquor of annual output 10000t caffeine, will cause heavy losses as not reclaiming.
Existing treatment process is the octanol extraction: octanol extraction-liquid caustic soda back extraction-concentrated-crystallization is centrifugal.The consumption of extraction process octanol is large, and chemical industry flavor is large, and COD of sewage, ammonia nitrogen are high; Operational path is long, and production unit is many, complicated operation; Consume steam 30t/d.
Therefore, seek a kind of new simple extraction process and substitute the octanol extraction process, reduce or remove the consumption of organic solvent, effectively improve the efficient of extracting, energy-saving and cost-reducing, be more significant.
Summary of the invention
Technical problem to be solved by this invention provides a kind of technique that reclaims the theophylline sodium salt from theophylline sodium salt mother liquor, improves the quality of products, and reduces production costs, and reduces and pollutes.
The present invention reclaims the technique of theophylline sodium salt from theophylline sodium salt mother liquor, it is characterized in that theophylline sodium salt mother liquor is neutralized with acid solution, neutralizer is through adsorption tower absorption, get through resolving again, wherein: acid solution adopts the dilute sulphuric acid of mass concentration 50-60%, pH is 4.5～6, and macroporous adsorbent resin is adopted in the agent of adsorption tower internal adsorption.
The polymeric adsorbent of suitable macropore is selected in the agent of adsorption tower internal adsorption, and such as the macroporous adsorbent resin of model LX-17, Xi'an blue dawn of science and technology is produced.
Be normal temperature absorption in the adsorption tower.
Adsorb completely, resolve.Desorbed solution adopts mass content at the liquid caustic soda solution of 3-4%, and the control flow is at 20000-25000L/h, and resolving keeps the pH value greater than 10.
Resolve completely, desorbed solution is directly used in first chemical industry order, removes first participation chemical reaction.
Advantage of the present invention:
1, not with an organic solvent, do not increase COD and ammonia-nitrogen content.Can reduce 110 tons of octanol consumptions every year, be worth 1.326 ten thousand yuan/tons=145.9 ten thousand yuan of 110 tons of *;
2, working cost is low, and working cost is lower than 50% of octanol extraction process; Water at low temperature reduces by 1.63 yuan/tons=193.2 ten thousand yuan of 300 days * of 3950 tons of/day * of consumption; Power consumption lowers ten thousand yuan of 0.6 yuan/kWh=49.5 of 300 days * of 2750kWh/ days *.
3, energy consumption is low, uses at steam especially and saves consumption more than 90%, reduces 3.6wt/y on the basis of original steam consumption 4wt/y, and annual steam saving is worth ten thousand yuan of 3.6wt*174.3 unit/t=627.5.
4, improve tea sodium and reclaim yield, can improve approximately more than 10% on the basis of extraction.
5, simple to operate, reduce labour intensity, improve Working environment (do not relate to solvent evaporates etc. to people's Health hazard), improve safety coefficient (not relating to the potential safety hazard that solvent etc. brings).
6, operation is carried out global optimization about the combination, realizes the purpose of green production.
Embodiment
The preparation of acid solution: the preparation mass concentration is the dilute sulphuric acid of 50-60%, and keeping pH is 4.5～6, can not add a small amount of sulfuric acid in scope or liquid caustic soda is adjusted in the scope;
The preparation of desorbed solution: add water in the liquid caustic soda basin, add mass content 30% liquid caustic soda again, open pressurized air and stir, sampling detects mass content at 3-4%, can suitably not add water or liquid caustic soda and regulate in scope; With 65-75 ℃ of steam intensification;
The preparation of regenerated liquid: add water in the dilute sulphuric acid basin, add mass content 30% sulfuric acid again, open pressurized air and stir, sampling detects mass content at 3-5%, can suitably not add water or sulfuric acid and regulate in scope.
In neutralizing tower, use the mother liquor of theophylline sodium salt in the acid solution and formation tea sodium neutralizer.Tea sodium neutralizer is squeezed in the absorption cat head with pump, drives tower valve and bleeder valve into, and the control flow carries out at the adsorption tower internal adsorption at 20000L-25000L/h, and sorbent material adopts the macroporous adsorbent resin (Xi'an blue dawn of science and technology is produced) of model LX-17.
Raffinate is collected decontaminated water factory and office reason by the sump tank.Adsorbing the complete pressurized air of opening dries up feed liquid in the adsorption column.Per hour residual row is taken a sample, detect the tea sodium content.The tea sodium content should be lower than 1000ppm in the residual liquid discharge liquid.
Adsorb complete, the desorbed solution for preparing is squeezed in the absorption cat head, drive the tower valve into, the control flow is resolved at 20000-25000L/h, resolving detects pH at any time, treats that pH is alkalescence, opens desorbed solution holding tank feed valve collection desorbed solution and enters the desorbed solution holding tank, sample presentation is delivered to first post (original process) by dehvery pump and uses after analyzing (reaching lower worker is that batching requires).PH13 above (sampling liquid is regulated pH decide terminal point) is transferred at any time discharging pipeline sampling valve sampling behind the adsorption tower of collection process, observes to have or not the crystallization of tea sodium, resolves terminal point to judge, separates out without tea sodium namely to reach parsing terminal point (routine operation).About total feed 30000L, close feed liquor alkali valve, close desorbed solution holding tank feed valve, with further part dilute solution access salkali waste tank, apply mechanically to get ready to go on foot when resolving, collect complete stopping and resolving.
The regenerated liquid that configures is squeezed in the absorption cat head, driven into the tower valve, flushing polymeric adsorbent (LX-17) is to neutrality or slightly acidic.About total feed 7000L, washing fluid enters sump.Regenerative process is taken a sample at any time and is transferred pH.The slightly acidic washing fluid enters the spent acid tank.
Embodiment 1:
According to above processing step, the tea sodium mass content 0.56% in the mother liquor, the tea sodium mass content 4% in the desorbed solution, waste liquid COD is 6000ppm, ammonia nitrogen 1000ppm.
Embodiment 2:
According to above processing step, the tea sodium mass content 0.6% in the mother liquor, tea sodium mass content 5 % in the desorbed solution, waste liquid COD is 6000ppm, ammonia nitrogen 1000ppm.
Claims (2)
1. technique that from theophylline sodium salt mother liquor, reclaims the theophylline sodium salt, it is characterized in that theophylline sodium salt mother liquor is neutralized with acid solution, neutralizer is through adsorption tower absorption, get through resolving again, wherein: acid solution adopts the dilute sulphuric acid of mass concentration 50-60%, pH is 4.5～6, macroporous adsorbent resin is adopted in the agent of adsorption tower internal adsorption, desorbed solution adopts mass content at the liquid caustic soda solution of 3-4%, the control flow is at 20000-25000L/h, resolving keeps the pH value greater than 10, and described macroporous adsorbent resin adopts the LX-17 macroporous adsorbent resin.
2. technique according to claim 1 is characterized in that the adsorption tower internal adsorption is normal temperature absorption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110160619 CN102250093B (en) | 2011-06-15 | 2011-06-15 | Process for recovering theophylline sodium salt from theophylline sodium salt mother liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110160619 CN102250093B (en) | 2011-06-15 | 2011-06-15 | Process for recovering theophylline sodium salt from theophylline sodium salt mother liquid |
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| CN102250093A CN102250093A (en) | 2011-11-23 |
| CN102250093B true CN102250093B (en) | 2013-04-17 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242313B (en) * | 2013-05-29 | 2015-04-01 | 石药集团新诺威制药股份有限公司 | Method for recovering sodium theophylline mother liquid |
| CN103992321B (en) * | 2014-06-09 | 2015-11-25 | 崇州合瑞科技有限公司 | A kind of preparation method of theophylline |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704818A (en) * | 2009-12-22 | 2010-05-12 | 陈学玺 | Method for extracting caffeine from methylated mother through adsorption separation |
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2011
- 2011-06-15 CN CN 201110160619 patent/CN102250093B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704818A (en) * | 2009-12-22 | 2010-05-12 | 陈学玺 | Method for extracting caffeine from methylated mother through adsorption separation |
Non-Patent Citations (3)
| Title |
|---|
| Qian-Li Zhang et al..Separation of caffeine and theophylline in poly(dimethylsiloxane) microchannel electrophoresis with electrochemical detection.《Journal of Chromatography A》.2005,第1098卷 * |
| Xien Hu et al..Theobromine and Caffeine Recovery with Solvent Extraction.《Separation Science and Technology》.2003,第38卷(第14期), * |
| 胡熙恩.咖啡因合成的绿色技术.《清华大学学报（自然科学版）》.2002,第42卷(第5期), * |
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