CN106517103B - Sodium hydrosulfite synthesizes continuous production method - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/64—Thiosulfates; Dithionites; Polythionates
- C01B17/66—Dithionites or hydrosulfites (S2O42-)
Abstract
The invention discloses a kind of sodium hydrosulfites to synthesize continuous production method, synthesis pot is used as a tubular reactor, raw material A E and ME are completed to be transferred to AE, ME basin with inert gas after preparing, it is added in the big dropwise addition pot of synthesis, the interior bottom insert canal that boils turns material to small dropwise addition pot is synthesized, it is relatively stable to turn to keep being added dropwise greatly during expecting material liquid level in pot, raw material A E and ME continue continuous uniform and are added in the big dropwise addition pot of synthesis, after the small dropwise addition pot of synthesis receives a batch materials, the second small pot that is added dropwise starts to receive from the big material that pot is added dropwise of synthesis, and so on；Small dropwise addition pot is from starting to receive material to terminal is reacted to, by raw material SO2‑CH3OH solution is continuously added to suitable speed until terminal, and after completing to keep the temperature maturation, blowing enters spare after drying process.Present invention omits the repeatable operation processes of reaction process, make building-up process serialization, and the consumption of sodium formate and sodium pyrosulfite is reduced while improving unit efficiency.
Description
Technical field
The invention belongs to the manufacturing technique method technical fields of sodium hydrosulfite, particularly relate to a kind of synthesis of sodium hydrosulfite
Continuous production method.
Background technology
Sodium hydrosulfite is also referred to as sodium dithionite, is a kind of white sand shape crystallization or pale yellow powder chemical article.Due to
Sulphur is in intermediate valence state, so sodium dithionite both has strong reducing property, also has strong oxidizing property.Mainly in textile industry, make
Paper industry is used as bleaching agent, and the toxic gases such as a large amount of heat and Liquor Hydrogen Peroxide, hydrogen sulfide can be discharged after being contacted with water.It is used extensively
In the fields such as the reproducibility dyeing of textile industry, reduction cleaning, bleaching and organic synthesis, wood pulp papermaking.
The method that sodium pyrosulfite is added from sodium formate method sodium hydrosulfite production technology in 1993 has in Guangdong at chemical industry
After limit company is successful, China colleague competitively imitates invariably.5 short years, China all use this method production insurance
Powder, but little in technical progress later, main the carrying in environmental protection and product quality of the technological progress of each manufacturer
Rise aspect.The synthetic reaction that sodium hydrosulfite produces is divided into tone pitch, heat preservation, big dropwise addition, droplet adduction guarantor when gap feeds intake production
The operating process such as warm maturation after often completing a batch of material, will repeat the above process, and technology innovation later makes little progress,
There is also problems for environmentally friendly aspect.
Continuity method production sodium hydrosulfite has been carried out in Japan.Mitsubishi gas sodium hydrosulfite device be with sodium formate solution,
Soda bath and methanol-SO2Solution produces sodium hydrosulfite, and after accurate calculation, synthesis is quantitatively adding with flowmeter, synthesis it is anti-
It is to have self-con-tained unit to answer pressure and temperature all.Synthesis turns a material, blowing, dry feed, compresses and washes and drying process is all strictly by journey
Sequence control carries out.
Sodium hydrosulfite serialization and automated production are realized on the basis of sodium pyrosulfite method, in China's sodium hydrosulfite industry
In, it is breakthrough technological progress.Synthesis serialization is then the core engineering for realizing sodium hydrosulfite serialization and automated production.In
The red Sifang Locomotive and Rolling Stock Co. Ltd., in salt Anhui has applied for the patent that a synthesis is continuously added dropwise greatly in October, 2013（Application number
201310501782.2）, from disclosure, core is led to when turning material to small dropwise addition pot after being added dropwise to complete greatly every time
Limitation is crossed to turn to expect that the material that big dropwise operation is completed is stayed certain volume by volumetric manner（2m3）Material as bottom material, then into
Row synthesis is big be added dropwise during be added dropwise the operation of AE, ME simultaneously, essence cannot calculate truly continuous.
Invention content
The present invention provides a kind of sodium hydrosulfite synthesis continuous production method, institute to overcome the shortcomings of the prior art
The synthesis serialization of meaning is will to synthesize pot to use as a tubular reactor, configures necessary equipment, establishes continuously to do and expect
Condition after, the repeatable operation process of reaction process is omitted, while greatly improving unit efficiency, reduce sodium formate and
The consumption of sodium pyrosulfite.
The present invention is achieved by the following technical solutions：A kind of sodium hydrosulfite synthesizes continuous production method, use AE,
ME、SO2-CH3OH solution, fluid conveying carrier and ethylene oxide are raw material, and AE is that the synthetic filtrate of dry product sodium formate and water are made into
Solution, ME is sulfur dioxide-methanol suspension with sodium pyrosulfite, and fluid conveying carrier is the first that mass fraction is 80%
Alcohol solution, sodium hydrosulfite synthesis continuous production method specifically include following steps：
（1）Stock：The preparation of AE and ME, mass fraction >=98% of HCOONa, sodium pyrosulfite are completed in configuration pot
Mass fraction >=60% of concentration, the mass fraction of sodium pyrosulfite is with SO2Meter, SO2-CH3OH,SO2Concentration >=370g/L carries
Body is the methanol that mass fraction is 78%~82%；
（2）Into bottom material：It is pressed into basin with inert gas, flowmeter is opened and is added dropwise into the AE of 1.5m3~2m3 to synthesis is big
Pot, starts to warm up；
（3）Tone pitch：Steam is opened when temperature rises to 75 DEG C~85 DEG C, pressure opens flow in 0.1 MPa~0.4MPa
It counts valve and SO is added to the big pot that is added dropwise2-CH3OH solution 20L~30L, are added a small amount of ethylene oxide, and adjust PH to 4.2~4.6；
（4）It is big to be added dropwise：After tone pitch 10min~20min, when temperature rises to 80 DEG C~86 DEG C, it is initially added into AE, ME, is made
PH stablizes 4.1~4.5, and pressure is 0.1 MPa~0.3MPa, and range estimation synthesis is big to be added dropwise in pot and reach 80% both after a batch of material,
Bottom insert canal continuously turns to expect to the tetra- small dropwise addition pots of A#~D# respectively in automatic open-top pot, and during turning material, raw material A E and ME continue
It is added to synthesis cauldron, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from synthesis
The big material that pot is added dropwise, and so on, the four small time being reacted to needed for terminal that pot is added dropwise is maintained always；
（5）Small dropwise addition：Temperature is controlled at 75 DEG C~85 DEG C, pressure 0.2Mpa~0.4Mpa is continuously added to SO2-CH3OH
Solution 10L~130L, PH control is 4.1~4.5, and carry out sodium hydrosulfite continuously generates reaction, improves the content of sodium hydrosulfite, range estimation
Synthesis feed liquid is limpid or analyzes the content of sodium thionyl in clear liquid, works as NaHSO3When≤10g/L, small completion of dropwise addition enters
Heat preservation operation；
（6）Heat preservation：Sampling analysis after heat preservation 10min, when pH value >=4.8, is fried under conditions of temperature is 75 DEG C~85 DEG C
When sample sodium hydrosulfite >=85%, heat preservation terminates；
（7）Cooling blowing：When temperature be 68 DEG C~75 DEG C, PH >=4.8, Na2S2O3Blowing when≤10g/L.
Step（2）In inert gas be nitrogen；Step（5）SO in small dropwise addition2-CH3After the rate of addition of OH is first fast
Slowly；Step（3）The flow of tone pitch ethylene oxide is according to the Na of analysis2S2O3Concentration is adjusted in time, be adjusted to ethylene oxide≤
5.6g/L；The flow of conveying AE and ME fluids is calculated as flow meter specially；In step（4）During big dropwise addition, whole process is added dropwise
It is complete to need 35min~40min/ batches, in step（5）During small dropwise addition, the operating process of small dropwise addition is 120min~150min/
Batch.
Carrier methanol plays the role of fluid transport, and entire building-up process realizes the chain adjusting control of temperature, flow and PH
System.The decomposition product that sodium hydrosulfite meets water is sodium hydrogensulfite and sodium thiosulfate.Sodium thiosulfate is the rush of the decomposition reaction again
Into agent, sodium hydrosulfite can be promoted further to decompose, therefore the matter of sodium thiosulfate in reaction system must be controlled using ethylene oxide
Concentration is measured, the mass concentration of sodium thiosulfate is made to be no more than 10 g/L.
AE, ME medium methanol and inhibit side reaction reagent ethylene oxide under the action of generate sodium hydrosulfite, carbon dioxide and
Water.The reaction principle of sodium hydrosulfite synthesis continuous production method of the present invention is as follows：
Overall reaction：1/2Na2S2O5+HCOONa+SO2 →Na2S2O4+CO2↑+1/2H2O
Side reaction：HCOOH+CH3OH → HCOOCH3+H2O
2Na2S2O4+H2O → Na2S2O3+ 2NaHSO3
Na2S2O3+H2COCH2+H2O→HOCH2CH2S2O3Na（Hydroxyethylthio sodium sulphate）+ NaOH
CH3OH+H2COCH2→HOCH2CH2OCH3（Glycol monoethyl ether）
NaHSO3+H2COCH2→HOCH2CH2SO3Na（Ethoxy sulphur sodium）
H2O+H2COCH2 → HOCH2CH2OH（Ethylene glycol）
The synthetic method of the present invention is changed to continuous dosing reaction by the former reaction that intermittently feeds intake, and can be not repeated to carry out to add bottom
Material, heating and tone pitch operation, save synthesis total time 30min~40min；After big dropwise addition process is continuous simultaneously, it can also save and turn
Expecting time 10min~15min, synthesising reacting time 40min~55min can be saved by adding up to, raising production efficiency 14.8%~
20.37%, synthesis procedure equipment investment 14.8%~20.37% is reduced under same size.
The present invention is a kind of feeding method of continuous synthetic reaction, makes it possible that reaction controlling automates, by accurate
Control feeds intake, and can make to contact more fully between material, entire synthetic reaction is more complete.Obtained product granularity is uniform, stable, thorough
Bottom, which changes interval synthetic method operation in current industry and fully relies on, manually to be controlled, and the product quality that arrives is irregular shows
Shape reduces or eliminates influence of the manual operations to synthetic reaction.
The synthesis serialization of the present invention can make same scale set efficiency improve 20% or so, raw material list compared with batch process
Consumption falls 8% or more on a year-on-year basis.After synthesizing serialization, since reaction is realized balanced, thus the tail gas discharged is also balanced, without controlling
It is forced enhanced processing facility because batch technology is unbalanced when managing exhaust gas, increases the phenomenon that investing.Wherein table one is to use
Continuously synthesis compares the method for the present invention with the consumption of raw materials that interval synthesizes.
Table one：Consumption of raw materials compares before and after synthesizing serialization
Note："+" indicates to improve in table, and "-" indicates to reduce.
The invention discloses a kind of synthesis continuous production method of sodium hydrosulfite, synthesis continuous process is will to synthesize pot to work as
Make a tubular reactor to use, under the conditions of ensureing technological parameter, raw material A E and ME is completed to prepare according to the ratio in preparation pot
It is transferred to AE, ME basin with inert gas afterwards, is added in the big dropwise addition pot of synthesis by delivery pump continuous uniform, pot is added dropwise when synthesis is big
Inside reach-determine volume（One batch of material）Afterwards, bottom insert canal continuously turns to expect to the tetra- small dropwise addition pots of A#~D# respectively in automatic open-top pot,
During turning material, material liquid level in dropwise addition pot greatly is kept to stablize relatively, raw material A E and ME continue continuous uniform and be added to synthesis greatly
It is added dropwise in pot, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from the big dropwise addition of synthesis
The material of pot, and so on, small dropwise addition pot, will be former under the conditions of ensureing technological parameter from starting to receive material to terminal is reacted to
Expect SO2-CH3OH solution is continuously added to suitable speed, always maintain it is four small be added dropwise pot be reacted to needed for terminal when
Between, after completing to keep the temperature maturation, blowing enters spare after drying process.
The beneficial effects of the invention are as follows：Sodium hydrosulfite synthesis continuous production method in the present invention is by the former reaction that intermittently feeds intake
It is changed to continuous dosing reaction, can be not repeated to carry out plus bottom material, heating, tone pitch operation, saving synthesize total time 40-55min,
Improve production efficiency 14.8-20.37%.Synthesis procedure equipment investment 14.8-20.37% is reduced under same size, is improved simultaneously
The irregular present situation of product quality, and yield can be improved, ratio of cutting down the consumption of raw materials can also effectively avoid prior art
It is unbalanced and be forced enhanced processing facility, increase the phenomenon that investing.Synthesis serialization in the present invention is will to synthesize pot to work as
Make tubular reactor to use, after configuring necessary equipment, establishing and can continuously do the condition expected, the weight of reaction process is omitted
Multiple operating process reduces the consumption of sodium formate and sodium pyrosulfite while greatly improving unit efficiency.
Description of the drawings
Fig. 1 is the flow chart of sodium hydrosulfite synthesis continuous production method of the present invention；
Fig. 2 is the schematic diagram that pot is synthesized in sodium hydrosulfite synthesis continuous production method of the present invention.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
As shown in Figure 1 to Figure 2, a kind of sodium hydrosulfite synthesizes continuous production method, uses AE, ME, SO2-CH3OH solution,
Fluid conveying carrier and ethylene oxide are raw material, and AE is the synthetic filtrate of dry product sodium formate and the solution that water is made into, and ME is with coke
Sulfur dioxide-methanol suspension of sodium sulfite, fluid conveying carrier are the methanol aqueous solution that mass fraction is 80%, sodium hydrosulfite
Synthesis continuous production method specifically includes following steps：
（1）Stock：The preparation of AE and ME, mass fraction >=98% of HCOONa, sodium pyrosulfite are completed in configuration pot
Mass fraction >=60% of concentration, the mass fraction of sodium pyrosulfite is with SO2Meter, SO2-CH3OH,SO2Concentration >=370g/L carries
Body is the methanol that mass fraction is 78%~82%；
（2）Into bottom material：It is pressed into basin with inert gas, flowmeter is opened and is added dropwise into the AE of 1.5m3~2m3 to synthesis is big
Pot, starts to warm up；
（3）Tone pitch：Steam is opened when temperature rises to 75 DEG C~85 DEG C, pressure opens flow in 0.1 MPa~0.4MPa
It counts valve and SO is added to the big pot that is added dropwise2-CH3The OH solution L of 20 L~30, are added a small amount of ethylene oxide, and adjust PH to 4.2~4.6；
（4）It is big to be added dropwise：After tone pitch 10min~20min, when temperature rises to 80 DEG C~86 DEG C, it is initially added into AE, ME, is made
PH stablizes 4.1~4.5, and pressure is 0.1 MPa~0.3MPa, and range estimation synthesis is big to be added dropwise in pot and reach 80% both after a batch of material,
Bottom insert canal continuously turns to expect to the tetra- small dropwise addition pots of A#~D# respectively in automatic open-top pot, and during turning material, raw material A E and ME continue
It is added to synthesis cauldron, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from synthesis
The big material that pot is added dropwise, and so on, the four small time being reacted to needed for terminal that pot is added dropwise is maintained always；
（5）Small dropwise addition：Temperature is controlled at 75 DEG C~85 DEG C, 0.2 Mpa of pressure~0.4Mpa is continuously added to SO2-CH3OH
Solution 10L~130L, PH control is 4.1~4.5, and carry out sodium hydrosulfite continuously generates reaction, improves the content of sodium hydrosulfite, range estimation
Synthesis feed liquid is limpid or analyzes the content of sodium thionyl in clear liquid, works as NaHSO3When≤10g/L, small completion of dropwise addition enters
Heat preservation operation；
（6）Heat preservation：Sampling analysis after heat preservation 10min, when pH value >=4.8, is fried under conditions of temperature is 75 DEG C~85 DEG C
When sample sodium hydrosulfite >=85%, heat preservation terminates；
（7）Cooling blowing：When temperature be 68 DEG C~75 DEG C, PH >=4.8, Na2S2O3Blowing when≤10g/L.
Step（1）In medium methanol be fluid conveying carrier, step（2）In inert gas be nitrogen；Step（5）It is small
SO in dropwise addition2-CH3The rate of addition of OH is first quick and back slow；Step（3）The flow of tone pitch ethylene oxide is according to analysis
Na2S2O3Concentration is adjusted in time, is adjusted to ethylene oxide≤5.6g/L；The flow of conveying AE and ME fluids is calculated as flow meter specially；
Step（4）During big dropwise addition, whole process, which drips, needs 35min~40min/ batches, in step（5）During small dropwise addition,
The operating process of small dropwise addition is 120min~150min/ batches.
Carrier methanol plays the role of fluid transport, and decomposition reaction inhibitor of the ethylene oxide as sodium hydrosulfite is entire to close
Temperature, the chain adjusting control of flow and PH are realized at process.The decomposition product that sodium hydrosulfite meets water is sodium hydrogensulfite and thio
Sodium sulphate.Sodium thiosulfate is the accelerating agent of the decomposition reaction again, sodium hydrosulfite can be promoted further to decompose, therefore must use epoxy
Ethane controls the mass concentration of sodium thiosulfate in reaction system, and the mass concentration of sodium thiosulfate is made to be no more than 10g/L.
AE, ME generate sodium hydrosulfite, carbon dioxide and water under the action of medium methanol and inhibition side reaction reagent ethylene oxide.
Embodiment 1：
Stock：Configuration quality score be 98% HCOONa, prepare mass fraction be 62% pyrosulfurous acid na concn with
SO2Meter, SO2-CH3OH,SO2Concentration >=370g/L, carrier methanol, mass fraction 78%；
Into bottom material：It is pressed into basin with inert gas, flowmeter is opened and pot is added dropwise into the AE of 1.8m3 or so to synthesis is big, open
Begin to heat up；
Tone pitch：Steam is opened when temperature rises to 76 DEG C, pressure is opened flowmeter valve and be added to the big pot that is added dropwise in 0.1MPa
SO2-CH3OH solution 25L, a certain amount of ethylene oxide, and PH is adjusted to 4.3；
It is big to be added dropwise：After tone pitch 10min~20min, when temperature rises to 81 DEG C~82 DEG C, it is initially added into AE, ME, PH is made to stablize
4.4~4.5, pressure is 0.2 MPa~0.25MPa, and big be added dropwise in pot of range estimation synthesis reaches 80%（One batch of material）Afterwards, automatic top
The interior bottom insert canal that boils continuously turns to expect, turn during expecting, raw material A E, ME continuously adds conjunction to the tetra- small dropwise addition pots of A#~D# respectively
At cauldron, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from the big dropwise addition pot of synthesis
Material, and so on；Always the four small time being reacted to needed for terminal that pot is added dropwise is maintained.
Small dropwise addition：Temperature is controlled at 82 DEG C~83 DEG C, pressure 0.2MPa~0.25MPa, is connected with rhythm first quick and back slow
It is continuous that SO is added2-CH34.5~4.6, carry out sodium hydrosulfite continuously generates reaction, improves sodium hydrosulfite for OH solution 100L, PH control
Content, range estimation synthesis feed liquid is limpid or analyzes the content of sodium thionyl in clear liquid, works as NaHSO3When≤10g/L, small dropwise addition
Terminate, is operated into heat preservation；
Heat preservation：Sampling analysis after 10min is kept the temperature, after pH value >=4.9, when frying sample sodium hydrosulfite >=85%, heat preservation terminates；
Cooling blowing：As 68 DEG C~75 DEG C of temperature, pH value >=4.9, Na2S2O3Blowing when≤10g/L.
Embodiment 2：
Stock：Configuration quality score be 99% HCOONa, prepare mass fraction be 64% pyrosulfurous acid na concn (with
SO2Meter), SO2-CH3OH,SO2Concentration >=370g/L, carrier methanol, mass fraction 79%；
Into bottom material：It is pressed into basin with inert gas, flowmeter is opened and pot is added dropwise into the AE of 2m3 or so to synthesis is big, start
Heating；
Tone pitch：Steam is opened when temperature rises to 80 DEG C, pressure opens flowmeter valve to big in 0.15MPa~0.2MPa
Pot is added dropwise, SO is added2-CH3OH solution 25L, a certain amount of ethylene oxide, and PH is adjusted to 4.4；
It is big to be added dropwise：After tone pitch 10min~20min, when temperature rises to 82 DEG C~83 DEG C, it is initially added into AE, ME, PH is made to stablize
4.3~4.4, pressure is 0.15 MPa~0.2MPa, and big be added dropwise in pot of range estimation synthesis reaches 80%（One batch of material）Afterwards, automatic top
The interior bottom insert canal that boils continuously turns to expect, turn during expecting, raw material A E, ME continuously adds conjunction to the tetra- small dropwise addition pots of A#~D# respectively
At cauldron, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from the big dropwise addition pot of synthesis
Material, and so on；Always the four small time being reacted to needed for terminal that pot is added dropwise is maintained.
Small dropwise addition：Temperature is controlled at 81 DEG C~82 DEG C, pressure 0.15MPa~0.2MPa, is connected with rhythm first quick and back slow
It is continuous that SO is added2-CH34.4~4.5, carry out sodium hydrosulfite continuously generates reaction, improves sodium hydrosulfite for OH solution 100L, PH control
Content, range estimation synthesis feed liquid is limpid or analyzes the content of sodium thionyl in clear liquid, works as NaHSO3When≤10g/L, small dropwise addition
Terminate, is operated into heat preservation；
Heat preservation：Sampling analysis after 10min is kept the temperature, after pH value >=4.9, when frying sample sodium hydrosulfite >=85%, heat preservation terminates.
Cooling blowing：When 68 DEG C~75 DEG C of temperature, PH >=4.9, Na2S2O3≤10g/L when blowing.
Finally it should be noted that the above content is merely illustrative of the technical solution of the present invention, rather than the present invention is protected
The limitation of range, those skilled in the art to technical scheme of the present invention carry out it is simple modification or equivalent replacement,
All without departing from the spirit and scope of technical solution of the present invention.
Claims (4)
1. a kind of sodium hydrosulfite synthesizes continuous production method, it is characterised in that：The sodium hydrosulfite synthesis continuous production method is adopted
With AE, ME, SO2-CH3OH solution and fluid conveying carrier are raw material, and the decomposition reaction inhibitor of sodium hydrosulfite is ethylene oxide, institute
The synthetic filtrate that AE is dry product sodium formate and the solution that water is made into are stated, the ME is that sulfur dioxide-methanol of sodium pyrosulfite is outstanding
Supernatant liquid, the fluid conveying carrier are the methanol aqueous solutions that mass fraction is 80%, and the sodium hydrosulfite synthesizes continuous production side
Method specifically includes following steps：
（1）Stock：The preparation of AE and ME, mass fraction >=98% of HCOONa, pyrosulfurous acid na concn are completed in configuration pot
Mass fraction >=60%, the mass fraction of sodium pyrosulfite is with SO2Meter, SO2-CH3OH,SO2Concentration >=370g/L, carrier are
The methanol aqueous solution that mass fraction is 78%~82%；
（2）Into bottom material：It is pressed into basin with inert gas, flowmeter is opened and pot is added dropwise into the AE of 1.5m3~2m3 to synthesis is big, open
Begin to heat up；
（3）Tone pitch：Steam is opened when temperature rises to 75 DEG C~85 DEG C, pressure opens flowmeter valve in 0.1 MPa~0.4MPa
SO is added to the big pot that is added dropwise2-CH3The OH solution L of 20 L~30, are added a small amount of ethylene oxide, and adjust pH to 4.2~4.6；
（4）It is big to be added dropwise：After tone pitch 10min~20min, when temperature rises to 80 DEG C~86 DEG C, it is initially added into AE, ME, keeps PH steady
4.1~4.5 are scheduled on, pressure is 0.1 MPa~0.3MPa, after reaching a 80% i.e. batch of material in the big dropwise addition pot of range estimation synthesis, automatically
Bottom insert canal continuously turns to expect to the tetra- small dropwise addition pots of A#~D# respectively in open-top pot, and during turning material, raw material A E and ME are continuously added
Pot is added dropwise to synthesis is big, after the small dropwise addition pot of synthesis receives a batch materials, second small dropwise addition pot starts to receive from synthesis
The big material that pot is added dropwise, and so on, the four small time being reacted to needed for terminal that pot is added dropwise is maintained always；
（5）Small dropwise addition：Temperature is controlled at 75 DEG C~85 DEG C, pressure 0.2MPa~0.4MPa is continuously added to SO2-CH3OH is molten
Liquid 10L~130L, pH control is 4.1~4.5, and carry out sodium hydrosulfite continuously generates reaction, improves the content of sodium hydrosulfite, range estimation
Synthesis feed liquid is limpid or analyzes the content of sodium thionyl in clear liquid, works as NaHSO3When≤10g/L, small completion of dropwise addition enters
Heat preservation operation；
（6）Heat preservation：The sampling analysis after heat preservation 10min under conditions of temperature is 75 DEG C~85 DEG C, when pH value >=4.8, fries sample guarantor
When dangerous powder >=85%, heat preservation terminates；
（7）Cooling blowing：When temperature be 68 DEG C~75 DEG C, pH >=4.8, Na2S2O3Blowing when≤10g/L；
The step（2）In inert gas be nitrogen, the step（3）The flow of tone pitch ethylene oxide is adjusted to≤5.6g/
L。
2. sodium hydrosulfite according to claim 1 synthesizes continuous production method, it is characterised in that：The step（5）Droplet
Add middle SO2-CH3The rate of addition of OH is first quick and back slow.
3. sodium hydrosulfite according to claim 1 synthesizes continuous production method, it is characterised in that：Convey the AE and ME streams
The flow of body is calculated as flow meter specially.
4. sodium hydrosulfite according to claim 1 synthesizes continuous production method, it is characterised in that：In step（4）It is big to be added dropwise
In the process, whole process, which drips, needs 35min~40min/ batches, in step（5）During small dropwise addition, the operation of small dropwise addition
Journey is 120min~150min/ batches.
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| 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 |
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