CN103482585B - Method and device for synthesizing sodium hydrosulfite - Google Patents
Method and device for synthesizing sodium hydrosulfite Download PDFInfo
- Publication number
- CN103482585B CN103482585B CN201310344817.6A CN201310344817A CN103482585B CN 103482585 B CN103482585 B CN 103482585B CN 201310344817 A CN201310344817 A CN 201310344817A CN 103482585 B CN103482585 B CN 103482585B
- Authority
- CN
- China
- Prior art keywords
- methyl alcohol
- reaction
- condenser
- preparation tank
- sulfur dioxide
- 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.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a process control method of the later period of a sodium hydrosulfite synthetic reaction, aiming at increasing the alcohol and water ratio at the later period of the synthetic reaction and reducing the occurrence probability of a decomposition reaction of sodium hydrosulfite. The method concretely comprises the steps of slowly dissolving solid sodium formate and sodium metabisulfite into a 60-70% methyl alcohol water solution according to the molar ratio of 2: 1; controlling the temperature of a reaction kettle to be 80-85 DEG C, controlling the pressure to be 0.15-0.25Mpa and controlling the pH to be 4.4-5.0; slowly adding liquid sulfur dioxide into the reaction kettle; after the raw material feeding is stopped, slowly adding the mixed solution of sulfur dioxide and methyl alcohol into the raw material; and additionally arranging a set of sulfur dioxide and methyl alcohol matching preparation device on the basis of original production equipment. According to the method and the device provided by the invention, the alcohol and water ratio of a reaction system can be increased, the side reaction is restricted, the purity of the product can be improved to more than 90%, and the safety risk in the production process is reduced.
Description
Technical field
The present invention relates to a kind of synthetic method and device of vat powder, be specially process control and the synthesizer of the later stage synthesis process of vat powder.
Background technology
Industrial production main raw material has sodium formiate, Sodium Pyrosulfite, sulfur dioxide liquid.Production technique is: first solid sodium formate and Sodium Pyrosulfite are dissolved in the mixed solvent of methyl alcohol, water, is controlling, under certain index such as temperature, pressure, pH, in reactor, constantly to add liquid SO
2carry out chemical reaction, finally synthesize vat powder, follow-uply obtain sodium hydrosulfite finished product through solid-liquid separation, washing, drying.Its principal reaction equation is: 2HCOONa+Na
2s
2o
5+ 2SO
2=2Na
2s
2o
4+ 2CO
2↑+H
2o.
As can be seen from synthetic chemistry reaction equation, methyl alcohol does not participate in reaction as solvent, and reaction process generates water, volatilization methyl alcohol, so reaction system alcohol water is than constantly reducing.Reaction later stage Sodium Hydrosulfite Content rises steadily, and alcohol water is than constantly reducing, and vat powder has the characteristic of meeting water decomposition, and reaction equation is: 2Na
2s
2o
4+ H
2o=2 NaHSO
3+ Na
2s
2o
3.Alcohol water is than lower, and decomposition reaction is faster, and violent decomposition also can cause reactor to blast fire failure, has both affected the content synthesizing vat powder, and has increased again the security risk of production.
Summary of the invention
The object of the present invention is to provide the process control in a kind of vat powder building-up reactions later stage, improve the alcohol water ratio in building-up reactions later stage, reduce the generation of vat powder decomposition reaction, and then improve the content of synthesis vat powder.
Concrete grammar is: a kind of synthetic method of vat powder, be that 2:1 is slowly dissolved in the methanol aqueous solution of 60 ~ 70% by solid sodium formate and Sodium Pyrosulfite with mol ratio, be 80-85 DEG C controlling the temperature of reactor, pressure is 0.15-0.25Mpa, PH is under 4.4-5.0, slowly add sulfur dioxide liquid to reactor, after stopping the feeding intake of raw material, slowly add the mixed solution of sulfurous gas and methyl alcohol.
Described sulfurous gas and methyl alcohol be that 1:1.5-3 is fed in reactor with volume ratio.
The flow that feeds intake of described sulfurous gas and methyl alcohol is 0.2-1.0m
3/ h, pressure is 0.15-0.25Mpa, and temperature of reaction is 80-85 DEG C.
Synthesizer in another object of the present invention is to provide synthesis of a kind of vat powder later stage treating processes to control.Specifically on the basis of original production equipment, newly-increased a set of sulfurous gas, methyl alcohol device for formulating, improve the content of synthesis vat powder.
Concrete process unit is: a kind of synthesizer of vat powder, comprises vat powder synthesis Preparation tank and ammonia condenser, passes into Preparation tank top after two canned-motor pumps in parallel of described Preparation tank bottom; Canned-motor pump is communicated with ammonia condenser inlet mouth by switch-valve through pressure pump respectively, simultaneously canned-motor pump respectively through pressure pump by switch-valve be communicated with workshop respectively, before workshop, under meter is set respectively; Condenser air outlet is communicated with Preparation tank top, condenser is arranged gaseous ammonia outlet, and arrange liquid ammonia outlet under condenser, described sulfur dioxide liquid reservoir is communicated with Preparation tank top through under meter respectively with methyl alcohol reservoir.
Described finished product by canned-motor pump through ammonia condenser circulate mixing, make product material be cooled to≤10 DEG C.
The invention has the advantages that: vat powder building-up reactions generates water, add the mixed solution of sulfurous gas and methyl alcohol in the building-up reactions later stage, the alcohol water ratio of reaction system can be improved, suppress the generation of side reaction, improve the purity of product to more than 90%, reduce the security risk in production process.
Accompanying drawing explanation
Fig. 1 is the synthesizer of vat powder, wherein, and 1. Preparation tank, 2. ammonia condenser, 2-1. ammonia condenser inlet mouth, 2-2. liquid ammonia exports, and 2-3. gaseous ammonia exports, 2-4. condenser air outlet, 3-1,2. canned-motor pump, 4-1,2. pressure pump, 5-1,2,3,4. under meter, 6. sulfurous gas reservoir, 7. methyl alcohol reservoir, 8-1,2. switch-valve.
Embodiment
Embodiment 1
A kind of synthetic method of vat powder, by solid sodium formate with to add S-WAT with mol ratio be that 2:1 is slowly dissolved in the methanol aqueous solution of 60 ~ 70%, be 80-85 DEG C controlling the temperature of reactor, pressure is 0.15-0.25Mpa, PH is under 4.4-5.0, slowly adds sulfur dioxide liquid to reactor, after stopping the feeding intake of raw material, slowly add the mixed solution that sulfurous gas and methyl alcohol take volume ratio as 1:1.5-3, the flow that feeds intake of sulfurous gas and methyl alcohol is 0.2-1.0m simultaneously
3/ h, pressure is 0.15-0.25Mpa, and temperature of reaction is 80-85 DEG C.
A synthesizer for vat powder, comprises vat powder synthesis Preparation tank 1 and ammonia condenser 2, and described Preparation tank 1 bottom two canned-motor pump 3-1 in parallel, pass into Preparation tank 1 top after 2; Canned-motor pump 3-1,2 respectively through pressure pump 4-1, and 2 are communicated with ammonia condenser inlet mouth 2-1 by switch-valve 8, simultaneously canned-motor pump 3-1, and 2 respectively through pressure pump 4-1,2 by switch-valve and respectively with workshop 8-1,2 connections, workshop 8-1, arranges under meter 5-3 before 2,4 respectively; Condenser air outlet 2-4 is communicated with Preparation tank 1 top, condenser 2 is arranged gaseous ammonia outlet 2-3, condenser arranges liquid ammonia outlet 2-2 for 2 times, and sulfur dioxide liquid reservoir 6 and methyl alcohol reservoir 7 are communicated with Preparation tank 1 top through under meter 5-1 and under meter 5-2 respectively.
Finished product by canned-motor pump 3-1,2 through ammonia condenser 2 circulate mixing, make product material be cooled to≤10 DEG C.
Method of the present invention and synthesizer are installed, vat powder purity can be provided to reach more than 90%, large industrial production can be widely used in.
Claims (2)
1. the synthetic method of a vat powder, be that 2:1 is slowly dissolved in the methanol aqueous solution of 60 ~ 70% by solid sodium formate and Sodium Pyrosulfite with mol ratio, be 80-85 DEG C controlling the temperature of reactor, pressure is 0.15-0.25MPa, pH is under 4.4-5.0, slowly sulfur dioxide liquid is added to reactor, it is characterized in that: after stopping the feeding intake of raw material, slowly add the mixed solution of sulfurous gas and methyl alcohol, described sulfurous gas and methyl alcohol be that 1:1.5-3 is fed in reactor with volume ratio, the flow that feeds intake of described sulfurous gas and methyl alcohol is 0.2-1.0m
3/ h, pressure is 0.15-0.25MPa, and temperature of reaction is 80-85 DEG C.
2. the synthesizer that the synthetic method of vat powder according to claim 1 is used, comprises vat powder synthesis Preparation tank (1) and ammonia condenser (2), passes into Preparation tank (1) top after two canned-motor pumps (3-1,3-2) in parallel of described Preparation tank (1) bottom; Canned-motor pump (3-1,3-2) respectively through pressure pump (4-1,4-2) be communicated with ammonia condenser inlet mouth (2-1) by switch-valve (8), simultaneously canned-motor pump (3-1,3-2) respectively through pressure pump (4-1,4-2) by switch-valve with respectively with workshop (8-1,8-2) be communicated with, workshop (8-1,8-2) is front arranges under meter (5-3,5-4) respectively; Condenser air outlet (2-4) is communicated with Preparation tank (1) top, condenser (2) is arranged gaseous ammonia outlet (2-3), liquid ammonia outlet (2-2) is set under condenser (2), it is characterized in that: sulfur dioxide liquid reservoir (6) and methyl alcohol reservoir (7) are communicated with Preparation tank (1) top through under meter (5-1) and under meter (5-2) respectively, finished product by canned-motor pump (3-1,3-2) through ammonia condenser (2) circulate mixing, make product material be cooled to≤10 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310344817.6A CN103482585B (en) | 2013-08-09 | 2013-08-09 | Method and device for synthesizing sodium hydrosulfite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310344817.6A CN103482585B (en) | 2013-08-09 | 2013-08-09 | Method and device for synthesizing sodium hydrosulfite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103482585A CN103482585A (en) | 2014-01-01 |
| CN103482585B true CN103482585B (en) | 2015-06-10 |
Family
ID=49823258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310344817.6A Active CN103482585B (en) | 2013-08-09 | 2013-08-09 | Method and device for synthesizing sodium hydrosulfite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103482585B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209350A (en) * | 2020-09-09 | 2021-01-12 | 茂名市广地化工有限公司 | Method and device for producing sodium hydrosulfite special for printing and dyeing industry |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100396598C (en) * | 2006-10-24 | 2008-06-25 | 烟台市金河保险粉厂有限公司 | Process for producing sodium formate using liquid sulfur dioxide and sodium pyrosulfite |
| CN102530883B (en) * | 2011-12-14 | 2013-10-23 | 烟台市金河保险粉厂有限公司 | Method for synthetizing sodium hydrosulfite |
-
2013
- 2013-08-09 CN CN201310344817.6A patent/CN103482585B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103482585A (en) | 2014-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103864099B (en) | The method of comprehensive utilization of a kind of cyanuric acid industrial gaseous waste and waste water | |
| CN101891261A (en) | Method for preparing ruthenium trichloride from coarse ruthenium powder | |
| CN103626240B (en) | Lower concentration complexity prepares the method for ruthenium trichloride containing ruthenium waste liquid | |
| CN104649884B (en) | Method and production device of preparing glyoxylic acid through catalytic oxidization of glyoxal by air with nitrogen oxide under normal pressure | |
| CN111285331A (en) | Method for preparing hydrobromic acid and sodium bromide from bromine-containing brine in short process | |
| CN103482585B (en) | Method and device for synthesizing sodium hydrosulfite | |
| CN103933831B (en) | A kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique | |
| CN203807156U (en) | Integrated chlorine dioxide preparation device | |
| CN104910031A (en) | Method for co-producing glycine and hydantoin, and apparatus thereof | |
| CN102491276B (en) | Method for producing sodium hypochlorite through adding alkali twice | |
| CN104177325A (en) | Trioxymethylene preparation apparatus and method thereof | |
| CN106631907B (en) | A kind of synthetic rubber accelerator systems and technique | |
| CN103387671B (en) | Dimethyldichlorosilane(DMCS) adopts Concentrated acid hydrolysis to prepare the technique of oligosiloxane | |
| CN103112835A (en) | Indirect bleaching method in concentrated nitric acid production process | |
| CN101343040B (en) | Liquefied chlorine flash evaporation purification preparation technique | |
| CN104108686B (en) | Pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride | |
| CN105293523A (en) | Continuous preparation method for production raw material ammonia water of ketazine process hydrazine hydrate | |
| CN104692408A (en) | Method for preparing propylene epoxide through propylene cyclization under catalysis of molybdenum/titanium silicalite molecular sieve | |
| CN104370783A (en) | Hydrogen sulfide recycling method and hydrogen sulfide recycling system for continuously producing mercaptoacetic acid by adopting sodium hydrosulfide method | |
| CN101559927B (en) | Green technology for synchronously producing chlorine dioxide and glyoxalic acid | |
| CN104891443A (en) | Pure chlorine dioxide preparing device and method realizing automatic gas-liquid separation | |
| CN103496722A (en) | Method for preparing high-purity sodium sulfite through supercritical hydrothermal reduction | |
| CN103951142A (en) | Treatment method and device for cyclohexanone ammoximation wastewater | |
| CN203346310U (en) | Pipeline-type reaction device for preparing trichloroisocyanuric acid | |
| CN203820663U (en) | Production system of 2-chlorine-4-nitrotoluene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |