CN108821950A - A kind of continuous neutralization reaction method of bisnaphthol production - Google Patents
A kind of continuous neutralization reaction method of bisnaphthol production Download PDFInfo
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- CN108821950A CN108821950A CN201810548073.2A CN201810548073A CN108821950A CN 108821950 A CN108821950 A CN 108821950A CN 201810548073 A CN201810548073 A CN 201810548073A CN 108821950 A CN108821950 A CN 108821950A
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- neutralization reaction
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- reaction kettle
- sodium sulfite
- kettle
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/01—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis
- C07C37/04—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis by substitution of SO3H groups or a derivative thereof
Abstract
The present invention relates to bisnaphthol production technical field, specially a kind of bisnaphthol produces continuous neutralization reaction method, and steps are as follows：The flow of sodium sulfite solution and naphthalene sulfonic acids is controlled, sodium sulfite solution inputs in three times, obtains final neutralizer after Pyatyi neutralization reaction and alkali are adjusted, during entire neutralization reaction, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：95-98：100, one to level Four neutralization reaction kettle top is discharged sulfur dioxide gas, collects for being acidified.Interior neutralization reaction temperature is 95-100 DEG C in neutralization reaction kettles at different levels, once：It is secondary：The mass ratio of sodium sulfite solution is 1-5 three times:1-4:1-2.Reaction unit includes sodium sulfite solution fluid reservoir, naphthalene sulfonic acids fluid reservoir, level-one, second level, three-level, level Four, Pyatyi neutralization reaction kettle and neutralizes flow container；Reaction process is stablized, and sulfur dioxide is persistently released, and uniform flow controls well, improves operating environment.
Description
Technical field
A kind of bisnaphthol of the present invention produces continuous neutralization reaction method, belongs to bisnaphthol production technical field.
Background technique
Bisnaphthol is a kind of broken thin slice of white or white powder chemical substance, is organic synthesis raw material and dyestuff intermediate,
For manufacturing tobias acid, butyric acid, betanaphthol -3- formic acid and azo dyes.It is also rubber antioxidant, dressing agent, fungicide, prevents
Mould dose, preservative, prevention and treatment helminth and anthelmintic drug etc. raw material.Fragrance, leather retanning agent, in terms of
There is application.
Neutralization reaction in bisnaphthol production uses the identical neutralization reaction kettle independent operation of 3 structures.After naphthalene is blown in hydrolysis
Naphthalene sulfonic acids with compressed air be pressed into neutralization reaction kettle in, be slowly added to concentration be 12% 80~90 DEG C of sodium sulfite solution with
Naphthalene sulfonic acids carries out neutralization reaction, and the sulfur dioxide for reacting generation is passed through the souring operation that acidification kettle is diluted material.It has reacted
After analysis qualification, corrective is moved to cooling bath with compressed air, after discharging, with steam blowing pipeline and is vented kettle
Interior overbottom pressure.Due to using batch production, sulfur dioxide is easy to be bled into workshop air, causes severe operational environment.Waterpower
Injection makes part sulfur dioxide be dissolved in the water when vacuumizing, and subsequent wastewater treatment difficulty is caused to increase, and needs in liquid alkaline progress
With increase production cost.Manual switch valve and observation visor, large labor intensity, operating environment are poor.
Summary of the invention
The present invention overcomes the shortcomings of the prior art, and the technical problem to be solved is that provide a kind of bisnaphthol production company
Continuous neutralization reaction method, reaction process are stablized, and sulfur dioxide is persistently released, and uniform flow controls well, can realize control at a distance
Room operation processed, improves operating environment.
In order to solve the above technical problems, the technical scheme adopted by the invention is that：A kind of bisnaphthol production is continuous to be neutralized instead
Induction method, steps are as follows：
The first step controls the flow of a sodium sulfite solution and naphthalene sulfonic acids by delivery pump and flowmeter, and sodium sulfite is molten
Liquid is continuously conveyed by reaction kettle top into level-one neutralization reaction kettle, and naphthalene sulfonic acids is continuously conveyed by reaction kettle side wall upper part into one
Grade neutralization reaction kettle；The liquid mixture obtained after level-one neutralization reaction is flowed continually out from level-one neutralization reaction bottom portion, is produced
Raw sulfur dioxide gas is discharged through level-one neutralization reaction kettle top；
Second step, the liquid mixture flowed continually out through level-one neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Second level neutralization reaction kettle, the flow of secondary sodium sulfite solution is controlled by delivery pump and flowmeter, and two Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into second level neutralization reaction kettle, and the liquid mixture obtained after second level neutralization reaction is from second level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through second level neutralization reaction kettle top；
Third step, the liquid mixture flowed continually out through second level neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Three-level neutralization reaction kettle controls the flow of sodium sulfite solution three times by delivery pump and flowmeter, and three Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into three-level neutralization reaction kettle, and the liquid mixture obtained after three-level neutralization reaction is from three-level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through three-level neutralization reaction kettle top；
4th step, the liquid mixture flowed continually out through three-level neutralization reaction bottom portion travel further into level Four neutralization reaction kettle,
The liquid mixture obtained after level Four neutralization reaction is flowed continually out from level Four neutralization reaction bottom portion, the sulfur dioxide gas of generation
Body is discharged through level Four neutralization reaction kettle top；
5th step, the liquid mixture flowed continually out through level Four neutralization reaction bottom portion travel further into Pyatyi neutralization reaction kettle,
The liquid mixture obtained after Pyatyi neutralization reaction is neutralized with sodium hydroxide solution adjustment pH value to after between 7-8 from Pyatyi
Reactor bottom flows continually out, and is passed through neutralization flow container.
During entire neutralization reaction, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：95-98：100.
The liquid mixture obtained after Pyatyi neutralization reaction, solution ph is between 1~2.
Described one sulfur dioxide gas being discharged to level Four neutralization reaction kettle top, collects and is further used for being acidified.
Interior neutralization reaction temperature is 95-100 DEG C in the neutralization reaction kettle at different levels.
Sodium sulfite solution：Secondary sodium sulfite solution：The mass ratio of sodium sulfite solution is 1-5 three times:
1-4:1-2。
A kind of continuous neutralization reaction device of bisnaphthol production, including sodium sulfite solution fluid reservoir, naphthalene sulfonic acids fluid reservoir, one
Grade neutralization reaction kettle, second level neutralization reaction kettle, three-level neutralization reaction kettle, level Four neutralization reaction kettle, Pyatyi neutralization reaction kettle and in
And flow container；
The sodium sulfite solution fluid reservoir passes through in sodium sulfite solution delivery pump and sodium sulfite solution flowmeter and level-one
It is connected with reaction kettle kettle top, the naphthalene sulfonic acids fluid reservoir passes through naphthalene sulfonic acids delivery pump and naphthalene sulfonic acids flowmeter and level-one neutralization reaction
The connection of kettle side wall upper part entrance, level-one neutralization reaction kettle outlet at bottom are connect with second level neutralization reaction kettle kettle top, in second level and anti-
Kettle outlet at bottom is answered to connect with three-level neutralization reaction kettle kettle top, three-level neutralization reaction kettle outlet at bottom and level Four neutralization reaction kettle kettle
Top connection, level Four neutralization reaction kettle outlet at bottom are connect with Pyatyi neutralization reaction kettle kettle top, Pyatyi neutralization reaction kettle outlet at bottom
Connection neutralizes flow container entrance；
The level-one, second level are provided with sodium sulfite solution flowmeter on three-level neutralization reaction kettle kettle top entrance pipe；
The level-one, second level, three-level and level Four neutralization reaction kettle kettle top are provided with sulfur dioxide gas outlet；
The Pyatyi neutralization reaction kettle kettle top is provided with alkali and adjusts mouth；
Agitating device is provided in the neutralization reaction kettle at different levels.
Compared to the prior art the present invention has the advantages that.
It in this serialization and compared with mode is neutralized with interval, neutralizes flow quantity and quality is guaranteed, sulfur dioxide release is flat
Surely, remote operation easy to accomplish, working condition are improved.Sodium sulfite is fed in three times, and charging will be lacked for the first time, guarantees naphthalene
Sulfonic acid is excessive, keeps the sodium naphthalene sulfonate crystal seed to be formed bigger, creates conditions for the filtering of subsequent sodium naphthalene sulfonate；Second of sodium sulfite
It is neutralization reaction Main Stage after charging, guarantees that a large amount of naphthalene sulfonic acids participate in reaction, sodium sulfite third time charging is to guarantee pH
Value is between 1 ~ 2.Compared with the continuous neutralization of charging simultaneously, sulfur dioxide releasing by parts, material is not easy to emit pot, reduces peace
The probability of happening of loopful guarantor's accident.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
In figure：1 it is sodium sulfite solution fluid reservoir, 2 be sodium sulfite solution delivery pump, 3 is sodium sulfite solution flow
Meter, 4 be naphthalene sulfonic acids fluid reservoir, 5 be naphthalene sulfonic acids delivery pump, 6 be naphthalene sulfonic acids flowmeter, 7 be level-one neutralization reaction kettle, 8 be second level
Neutralization reaction kettle, 9 be three-level neutralization reaction kettle, 10 be level Four neutralization reaction kettle, 11 be Pyatyi neutralization reaction kettle, 12 be neutralizer
Tank, 13 are that sulfur dioxide gas exports, 14 be that alkali adjusts mouth.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
The continuous neutralization reaction device of a kind of bisnaphthol production, which is characterized in that including sodium sulfite solution fluid reservoir 1, naphthalene
Sulfonic acid fluid reservoir 4, level-one neutralization reaction kettle 7, second level neutralization reaction kettle 8, three-level neutralization reaction kettle 9, level Four neutralization reaction kettle 10,
Pyatyi neutralization reaction kettle 11 and neutralization flow container 12；
1 tank of sodium sulfite solution liquid storage passes through sodium sulfite solution delivery pump 2 and sodium sulfite solution flowmeter 3 and level-one
The connection of 7 kettle top of neutralization reaction kettle, the naphthalene sulfonic acids fluid reservoir 4 pass through in naphthalene sulfonic acids delivery pump 5 and naphthalene sulfonic acids flowmeter 6 and level-one
It being connected with 7 side wall upper part entrance of reaction kettle, 7 outlet at bottom of level-one neutralization reaction kettle is connect with 8 kettle top of second level neutralization reaction kettle, and two
8 outlet at bottom of grade neutralization reaction kettle is connect with 9 kettle top of three-level neutralization reaction kettle, 9 outlet at bottom of three-level neutralization reaction kettle and level Four
The connection of 10 kettle top of neutralization reaction kettle, 10 outlet at bottom of level Four neutralization reaction kettle are connect with 11 kettle top of Pyatyi neutralization reaction kettle, Pyatyi
The connection of 11 outlet at bottom of neutralization reaction kettle neutralizes 12 entrance of flow container；
The level-one, second level are provided with sodium sulfite solution flowmeter 3 on three-level neutralization reaction kettle kettle top entrance pipe；
The level-one, second level, three-level and level Four neutralization reaction kettle kettle top are provided with sulfur dioxide gas outlet 13；
The Pyatyi neutralization reaction kettle kettle top is provided with alkali and adjusts mouth 14；
Agitating device is provided in the neutralization reaction kettle at different levels.
A kind of continuous neutralization reaction method of bisnaphthol production, steps are as follows：
The first step controls the flow of a sodium sulfite solution and naphthalene sulfonic acids by delivery pump and flowmeter, and sodium sulfite is molten
Liquid is continuously conveyed by reaction kettle top into level-one neutralization reaction kettle, and naphthalene sulfonic acids is continuously conveyed by reaction kettle side wall upper part into one
Grade neutralization reaction kettle；The liquid mixture obtained after level-one neutralization reaction is flowed continually out from level-one neutralization reaction bottom portion, is produced
Raw sulfur dioxide gas is discharged through level-one neutralization reaction kettle top；
Second step, the liquid mixture flowed continually out through level-one neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Second level neutralization reaction kettle, the flow of secondary sodium sulfite solution is controlled by delivery pump and flowmeter, and two Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into second level neutralization reaction kettle, and the liquid mixture obtained after second level neutralization reaction is from second level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through second level neutralization reaction kettle top；
Third step, the liquid mixture flowed continually out through second level neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Three-level neutralization reaction kettle controls the flow of sodium sulfite solution three times by delivery pump and flowmeter, and three Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into three-level neutralization reaction kettle, and the liquid mixture obtained after three-level neutralization reaction is from three-level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through three-level neutralization reaction kettle top；
4th step, the liquid mixture flowed continually out through three-level neutralization reaction bottom portion travel further into level Four neutralization reaction kettle,
The liquid mixture obtained after level Four neutralization reaction is flowed continually out from level Four neutralization reaction bottom portion, the sulfur dioxide gas of generation
Body is discharged through level Four neutralization reaction kettle top；
5th step, the liquid mixture flowed continually out through level Four neutralization reaction bottom portion travel further into Pyatyi neutralization reaction kettle,
The liquid mixture obtained after Pyatyi neutralization reaction is neutralized with sodium hydroxide solution adjustment pH value to after between 7-8 from Pyatyi
Reactor bottom flows continually out, and is passed through neutralization flow container.
Described one sulfur dioxide gas being discharged to level Four neutralization reaction kettle top, collects and is further used for being acidified.
Embodiment 1
During above-mentioned entire neutralization reaction, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：97：100.
The liquid mixture obtained after Pyatyi neutralization reaction, solution ph 1.5.
Interior neutralization reaction temperature is 95 DEG C in the neutralization reaction kettle at different levels.
Sodium sulfite solution：Secondary sodium sulfite solution：The mass ratio of sodium sulfite solution is 5 three times:4:
2。
Embodiment 2
During above-mentioned entire neutralization reaction, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：95：100.
The liquid mixture obtained after Pyatyi neutralization reaction, solution ph 1.
Interior neutralization reaction temperature is 98 DEG C in the neutralization reaction kettle at different levels.
Sodium sulfite solution：Secondary sodium sulfite solution：The mass ratio of sodium sulfite solution is 1 three times:1:
1。
Embodiment 3
During above-mentioned entire neutralization reaction, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：98：100.
The liquid mixture obtained after Pyatyi neutralization reaction, solution ph 2.
Interior neutralization reaction temperature is 100 DEG C in the neutralization reaction kettle at different levels.
Sodium sulfite solution：Secondary sodium sulfite solution：The mass ratio of sodium sulfite solution is 3 three times:2:
1。
The embodiment of the present invention is explained in detail above in conjunction with attached drawing, but the present invention is not limited to above-mentioned implementations
Example, within the knowledge of a person skilled in the art, can also make without departing from the purpose of the present invention
Various change out.
Claims (7)
1. a kind of bisnaphthol produces continuous neutralization reaction method, which is characterized in that steps are as follows：
The first step controls the flow of a sodium sulfite solution and naphthalene sulfonic acids by delivery pump and flowmeter, and sodium sulfite is molten
Liquid is continuously conveyed by reaction kettle top into level-one neutralization reaction kettle, and naphthalene sulfonic acids is continuously conveyed by reaction kettle side wall upper part into one
Grade neutralization reaction kettle；The liquid mixture obtained after level-one neutralization reaction is flowed continually out from level-one neutralization reaction bottom portion, is produced
Raw sulfur dioxide gas is discharged through level-one neutralization reaction kettle top；
Second step, the liquid mixture flowed continually out through level-one neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Second level neutralization reaction kettle, the flow of secondary sodium sulfite solution is controlled by delivery pump and flowmeter, and two Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into second level neutralization reaction kettle, and the liquid mixture obtained after second level neutralization reaction is from second level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through second level neutralization reaction kettle top；
Third step, the liquid mixture flowed continually out through second level neutralization reaction bottom portion, is continuously inputted by reaction kettle side wall upper part
Three-level neutralization reaction kettle controls the flow of sodium sulfite solution three times by delivery pump and flowmeter, and three Sodium Thiosulfates are molten
Liquid is continuously conveyed by reaction kettle top into three-level neutralization reaction kettle, and the liquid mixture obtained after three-level neutralization reaction is from three-level
Neutralization reaction bottom portion flows continually out, and the sulfur dioxide gas of generation is discharged through three-level neutralization reaction kettle top；
4th step, the liquid mixture flowed continually out through three-level neutralization reaction bottom portion travel further into level Four neutralization reaction kettle,
The liquid mixture obtained after level Four neutralization reaction is flowed continually out from level Four neutralization reaction bottom portion, the sulfur dioxide gas of generation
Body is discharged through level Four neutralization reaction kettle top；
5th step, the liquid mixture flowed continually out through level Four neutralization reaction bottom portion travel further into Pyatyi neutralization reaction kettle,
The liquid mixture obtained after Pyatyi neutralization reaction is neutralized with sodium hydroxide solution adjustment pH value to after between 7-8 from Pyatyi
Reactor bottom flows continually out, and is passed through neutralization flow container.
2. a kind of bisnaphthol as described in claim 1 produces continuous neutralization reaction method, which is characterized in that entire neutralization reaction
In the process, the molar ratio of sodium sulfite solution and naphthalene sulfonic acids is：95-98：100.
3. a kind of bisnaphthol as described in claim 1 produces continuous neutralization reaction method, which is characterized in that described through in Pyatyi
With the liquid mixture obtained after reaction, solution ph is between 1~2.
4. a kind of bisnaphthol as described in claim 1 produces continuous neutralization reaction method, which is characterized in that described one to level Four
The sulfur dioxide gas of neutralization reaction kettle top discharge, collects and is further used for being acidified.
5. a kind of bisnaphthol as described in claim 1 produces continuous neutralization reaction method, which is characterized in that the neutralizations at different levels
Interior neutralization reaction temperature is 95-100 DEG C in reaction kettle.
6. a kind of bisnaphthol as described in claim 1 produces continuous neutralization reaction method, which is characterized in that a sulfurous
Acid sodium solution：Secondary sodium sulfite solution：The mass ratio of sodium sulfite solution is 1-5 three times:1-4:1-2.
7. a kind of bisnaphthol produces continuous neutralization reaction device, which is characterized in that including sodium sulfite solution fluid reservoir, naphthalene sulfonic acids
It is fluid reservoir, level-one neutralization reaction kettle, second level neutralization reaction kettle, three-level neutralization reaction kettle, level Four neutralization reaction kettle, in Pyatyi and anti-
It answers kettle and neutralizes flow container；
The sodium sulfite solution fluid reservoir passes through in sodium sulfite solution delivery pump and sodium sulfite solution flowmeter and level-one
It is connected with reaction kettle kettle top, the naphthalene sulfonic acids fluid reservoir passes through naphthalene sulfonic acids delivery pump and naphthalene sulfonic acids flowmeter and level-one neutralization reaction
The connection of kettle side wall upper part entrance, level-one neutralization reaction kettle outlet at bottom are connect with second level neutralization reaction kettle kettle top, in second level and anti-
Kettle outlet at bottom is answered to connect with three-level neutralization reaction kettle kettle top, three-level neutralization reaction kettle outlet at bottom and level Four neutralization reaction kettle kettle
Top connection, level Four neutralization reaction kettle outlet at bottom are connect with Pyatyi neutralization reaction kettle kettle top, Pyatyi neutralization reaction kettle outlet at bottom
Connection neutralizes flow container entrance；
The level-one, second level are provided with sodium sulfite solution flowmeter on three-level neutralization reaction kettle kettle top entrance pipe；
The level-one, second level, three-level and level Four neutralization reaction kettle kettle top are provided with sulfur dioxide gas outlet；
The Pyatyi neutralization reaction kettle kettle top is provided with alkali and adjusts mouth；
Agitating device is provided in the neutralization reaction kettle at different levels.
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| CN201810548073.2A CN108821950A (en) | 2018-05-31 | 2018-05-31 | A kind of continuous neutralization reaction method of bisnaphthol production |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078715A (en) * | 1992-05-21 | 1993-11-24 | 蔡宪元 | The joint process of methyl naphthol and ethyl naphthol |
| CN101781172A (en) * | 2010-01-04 | 2010-07-21 | 曲靖众一精细化工股份有限公司 | Novel process for efficiently and continuously synthesizing 2-naphthol |
| CN103626637A (en) * | 2013-12-11 | 2014-03-12 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of 2-naphthol |
| CN104592062A (en) * | 2015-02-16 | 2015-05-06 | 曲靖众一合成化工有限公司 | Method and device for continuously neutralizing beta-naphthalene sulfonic acid and comprehensively recycling waste gas |
| CN206051895U (en) * | 2016-08-19 | 2017-03-29 | 浙江龙盛化工研究有限公司 | A kind of continuous neutralization device of LOMAR PWA EINECS 246-676-2 or derivatives thereof |
-
2018
- 2018-05-31 CN CN201810548073.2A patent/CN108821950A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078715A (en) * | 1992-05-21 | 1993-11-24 | 蔡宪元 | The joint process of methyl naphthol and ethyl naphthol |
| CN101781172A (en) * | 2010-01-04 | 2010-07-21 | 曲靖众一精细化工股份有限公司 | Novel process for efficiently and continuously synthesizing 2-naphthol |
| CN103626637A (en) * | 2013-12-11 | 2014-03-12 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of 2-naphthol |
| CN104592062A (en) * | 2015-02-16 | 2015-05-06 | 曲靖众一合成化工有限公司 | Method and device for continuously neutralizing beta-naphthalene sulfonic acid and comprehensively recycling waste gas |
| CN206051895U (en) * | 2016-08-19 | 2017-03-29 | 浙江龙盛化工研究有限公司 | A kind of continuous neutralization device of LOMAR PWA EINECS 246-676-2 or derivatives thereof |
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