CN108752244A - A kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide - Google Patents
A kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide Download PDFInfo
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- CN108752244A CN108752244A CN201810482441.8A CN201810482441A CN108752244A CN 108752244 A CN108752244 A CN 108752244A CN 201810482441 A CN201810482441 A CN 201810482441A CN 108752244 A CN108752244 A CN 108752244A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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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
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Abstract
The invention discloses a kind of techniques producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, sulfonating reaction is carried out using Waste Sulfuric Acid and naphthalene, it is subsequently passed sulfur trioxide, it is reacted with water by sulfur trioxide and generates sulfuric acid sulfonating reaction to positive direction progress, continue sulfonating reaction with unreacted naphthalene in system, impurity enters granulation barrel removing with three fractions in Waste Sulfuric Acid；This process can improve the yield of beta naphthal, greatly reduce in production process and wastewater flow rate, and realize that industrial waste sulfuric acid directly utilizes.Industrial waste sulfuric acid, which directly recycles, can realize that the green production of country's promotion requires and reduce enterprise operations and production cost.
Description
Technical field
The present invention relates to dangerous wastes to recycle and beta naphthal production technical field, and in particular to a kind of to utilize Waste Sulfuric Acid and three
The technique of the double sulfonation technology production beta naphthals of sulfur oxide.
Background technology
China beta naphthal domestic consumption constitute approximately as：Dyestuff intermediate account for 60%, rubber chemicals account for 20%, dyestuff and
Pigment accounts for 10%, other account for 10%.
Dyestuff intermediate is the maximum consumption market of China's beta naphthal, major reason be dyestuff intermediate production into
The global transfer of row, such as 2,3- acid, J acid, G acid, R acid, azoic coupling component AS etc. are the important intermediate exported products in China, close several
Annual export volume accounts for the half or so of gross domestic product.Therefore China has become world's beta naphthal and mainly produces, consumes and export
State.But that all there is unit consumption to some extent is high for the production of beta naphthal, quantity of three wastes is big, contains to some extent in finished product and does not need
Other isomers and impurity etc..Therefore in facing the increasingly fierce market competition of dyestuff and pigment intermediates, technique is continuously improved,
Product quality is improved, reduce the three wastes has great practical benefit to the research and development of beta naphthal new technique for synthesizing.
In the industrial production, Waste Sulfuric Acid mainly has following source：Pesticide, ammonium sulfate and calcium superphosphate, titanium dioxide, oil work
The production process of industry gasoline, lubricating oil；The processes such as nitrification, sulfonation, esterification, alkylation, catalysis and the drying of organic matter；Steel acid
It washes and the processes such as gas dry.Waste Sulfuric Acid is broadly divided into organic Waste Sulfuric Acid and inorganic Waste Sulfuric Acid by the difference of its impurities.According to
Estimation, inorganic Waste Sulfuric Acid accounts for about 35% in China's Waste Sulfuric Acid at present, and organic Waste Sulfuric Acid accounts for 65%；With China's sulphuric acid output and table
The increasingly increase of consumption is seen, the quantum of output of Waste Sulfuric Acid is also rising year by year.Waste Sulfuric Acid has environment as production waste liquid
Great harm is vigorously advocating the today for recycling sustainable economy as China's sulfuric acid demand increasingly increases, Waste Sulfuric Acid
Processing and recycling will be as a research topics with important practical usage.
Industrial waste sulfuric acid is generally subjected to different degrees of dilution and pollution, thus generally can not directly return to original production
System recycles.But for certain production processes, if the concentration of this Waste Sulfuric Acid is suitable, impurities are to its work
Skill process and product quality have no significant effect again, then this Waste Sulfuric Acid can be directly used in the production process.Spent acid integrates
It utilizes, not only contributes to improve the sulfuric acid situation that supply falls short of demand, but also the processing cost of Waste Sulfuric Acid can be saved, apparent economy can be received
Benefit.
The acetylene gas of certain coal chemical industry group concentrated sulfuric acid washing, purifying, generates a large amount of Waste Sulfuric Acid every year.This part is useless
Sulfuric acid is the dark brown thick liquid of stabilization, brown or light brown after dilution, and without apparent suspended matter, key component is sulphur
Acid 90%~92%, remaining is organic matter and solid content etc..The Waste Sulfuric Acid is due to impure more, it is difficult to directly utilizes, if
Direct emission is discharged after simple neutralisation treatment, can cause environmental pollution.If being recycled both to this Waste Sulfuric Acid
Environmental pollution, and recyclable a part of sulfuric acid resource can be mitigated significantly, there is certain economic benefit and environmental benefit.
Sulfonating agent is mainly made using the concentrated sulfuric acid or oleum both at home and abroad at present, also has and naphthalene is carried out using gas phase sulfur trioxide
Sulfonating reaction.However, will produce a large amount of acid pickle when using the concentrated sulfuric acid or oleum sulfonated naphthalene, cause serious pollution to the environment；
Meanwhile although the generation that naphthalene sulfonation can reduce the consumption and reduction spent acid of sulfonating agent, phase are carried out using gaseous sulfur trioxide
The corollary equipment investment answered is higher, and exhaust emissions amount is big；For these, make according to Waste Sulfuric Acid and gaseous sulfur trioxide collocation
With the problem of then both having solved the difficult of Waste Sulfuric Acid and recycled, while exhaust emissions amount and equipment corrosion can also be reduced.
Invention content
The purpose of the present invention is to provide a kind of works producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide
Skill, application process include the following steps,
(1) refined naphthalene is added in reaction kettle, is heated to 135 DEG C while stirring, Waste Sulfuric Acid is added dropwise, 40min is persistently added dropwise,
Then it is 139-141 DEG C to maintain the temperature of mixed solution, and sulfur trioxide is slowly introducing into reaction kettle, is passed through the time and is
1.5h；
(2) when mixed solution temperature rises to 162-164 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down.
(3) when mixed solution temperature drops to 129-131 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows
Naphthalene continues 4h；
(4) be slowly added to sodium sulfite solution into reaction kettle, entire adition process duration 50min, then cool down after
Filter obtains 2- sodium naphthalene sulfonate solids.
(5) piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320-340 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Preferably, include following parts by weight raw material, 110~130 parts of refined naphthalenes, 60~80 parts of sulfur wastes in above-mentioned preparation process
Acid, 25~35 parts of sulfur trioxides, 150~200 parts of sodium sulfite solutions and 50~65 parts of piece alkali.
Preferably, sulfuric acid mass fraction is 96% in above-mentioned steps (1) Waste Sulfuric Acid.
Preferably, it is realized and is cooled down by natural cooling in above-mentioned steps (2).
Preferably, reaction temperature is 129-130 DEG C in above-mentioned steps (3).
Preferably, above-mentioned steps (4) sulfite sodium solution sulfite sodium mass fraction is 18%.
Preferably, above-mentioned steps (5) heating temperature is 321-339 DEG C.
Advantageous effect of the present invention：
The present invention carries out sulfonating reaction first with Waste Sulfuric Acid and naphthalene, is subsequently passed sulfur trioxide, passes through sulfur trioxide and water
Reaction generates sulfuric acid sulfonating reaction and is carried out to positive direction, continues sulfonating reaction with unreacted naphthalene in system, in Waste Sulfuric Acid
Impurity enters granulation barrel with three fractions and removes；This process can improve the yield of beta naphthal, greatly reduce in production process
And wastewater flow rate, and realize that industrial waste sulfuric acid directly utilizes.Industrial waste sulfuric acid, which directly recycles, can realize the green of country's promotion
Color production requirement, and enterprise operations and production cost can be reduced.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the implementation of the present invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
The every other embodiment that those of ordinary skill is obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1：
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 65 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 141 DEG C then to maintain the temperature of mixed solution, and 26 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 164 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 131 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) 165 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 60 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 340 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 90% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 2
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 65 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 140 DEG C then to maintain the temperature of mixed solution, and 26 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 163 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 130 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) 165 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 60 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 325 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 92% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 3
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 65 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 26 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 164 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) 165 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 60 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 330 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 94% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 4
Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide is utilized to produce the technique of beta naphthals the present invention provides a kind of,
Application process includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 65 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 26 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 162 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) 165 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 60 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 96% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 5
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 65 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 140 DEG C then to maintain the temperature of mixed solution, and 26 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 163 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 130 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) 165 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 60 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 335 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 98% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 6：
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, the 68 parts of sulfuric acid that give up are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 29 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 162 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h
(4) 174 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 58 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 96% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 7：
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 130 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 78 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 30 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 162 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h
(4) 160 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 56 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 96% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 8：
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 130 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 70 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 33 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 162 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h
(4) 190 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 65 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 96% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Embodiment 9：
The present invention provides a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, applications
Method includes the following steps,
(1) 120 parts of refined naphthalenes are added in reaction kettle, are heated to 135 DEG C while stirring, 75 parts of Waste Sulfuric Acids are added dropwise, continued
40min is added dropwise, it is 139 DEG C then to maintain the temperature of mixed solution, and 32 parts of sulfur trioxides are slowly introducing into reaction kettle, is passed through
Time is 1.5h；
(2) when mixed solution temperature rises to 162 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h
(4) 180 parts of sodium sulfite solutions are slowly added into reaction kettle, then entire adition process duration 50min cools down
It refilters to obtain 2- sodium naphthalene sulfonate solids.
(5) 55 parts of piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320 DEG C, obtains the piece aqueous slkali of 2- sodium naphthalene sulfonates, it is molten
Liquid obtains beta naphthal product through dilution, acidification, drying and distillation.
Sulfuric acid mass fraction is 96% in step (1) Waste Sulfuric Acid.
It is realized and is cooled down by natural cooling in the step (2).
Step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
Influence of the sulfuric acid score to beta naphthal yield in 1 Waste Sulfuric Acid quality of table
Choose 120 parts of refined naphthalenes, 65 parts of Waste Sulfuric Acids, 26 parts of sulfur trioxides, 18% sodium sulfite and 165 parts of piece alkali, according to
Embodiment 1-5 prepares beta naphthal, and measures beta naphthal yield, and the results are shown in Table 1.As shown in Table 1, beta naphthal yield is with sulphur
Sour mass fraction increase first increases to be reduced afterwards, and when sulfuric acid mass fraction is 96%, beta naphthal yield highest is 83.05%.
The sulfuric acid that mass fraction is 96% is chosen, prepares beta naphthal according to embodiment 4,6-9, and measure beta naphthal yield,
As shown in table 2.As shown in Table 2, directly sulfonation is carried out using Waste Sulfuric Acid prepare beta naphthal, beta naphthal average yield is more than 87%,
Highest yield reaches 89%.
2 beta naphthal yield of the present invention of table
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, it will be understood by those of ordinary skill in the art that：It still can be to aforementioned each implementation
Technical solution recorded in example is modified or equivalent replacement of some of the technical features；And these modification or
It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide, which is characterized in that its technique packet
Include following steps：
(1) refined naphthalene is added in reaction kettle, is heated to 135 DEG C while stirring, Waste Sulfuric Acid is added dropwise, 40min is persistently added dropwise, then
It is 139-141 DEG C to maintain the temperature of mixed solution, and sulfur trioxide is slowly introducing into reaction kettle, and it is 1.5h to be passed through the time；
(2) when mixed solution temperature rises to 162-164 DEG C in reaction kettle, 3h is kept the temperature, is then cooled down；
(3) when mixed solution temperature drops to 129-131 DEG C in reaction kettle, into reaction kettle being continuously passed through steam blows naphthalene, holds
Continuous 4h；
(4) sodium sulfite solution, entire adition process duration 50min are slowly added into reaction kettle, then cooling refilters
To 2- sodium naphthalene sulfonate solids；
(5) piece alkali and 2- sodium naphthalene sulfonates are mixed, is heated to 320-340 DEG C, obtain the piece aqueous slkali of 2- sodium naphthalene sulfonates, solution warp
Dilution, acidification, dry and distillation obtain beta naphthal product.
2. utilizing the technique of Waste Sulfuric Acid and the double sulfonation technology production beta naphthals of sulfur trioxide, feature according to claim 1
Be, the production technology include following parts by weight raw material, 110~130 parts of refined naphthalenes, 60~80 parts of Waste Sulfuric Acids, 25~35 parts
Sulfur trioxide, 150~200 parts of sodium sulfite solutions and 50~65 parts of piece alkali.
3. utilizing the technique of Waste Sulfuric Acid and the double sulfonation technology production beta naphthals of sulfur trioxide, feature according to claim 1
It is, sulfuric acid mass fraction is 96% in the Waste Sulfuric Acid that the step (1) uses.
4. utilizing the technique of Waste Sulfuric Acid and the double sulfonation technology production beta naphthals of sulfur trioxide, feature according to claim 1
It is, is realized and cooled down by natural cooling in the step (2).
5. a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide according to claim 1,
It is characterized in that, reaction temperature is 129-130 DEG C in the step (3).
6. a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide according to claim 1,
It is characterized in that, step (4) the sulfite sodium solution sulfite sodium mass fraction is 18%.
7. a kind of technique producing beta naphthal using Waste Sulfuric Acid and the double sulfonation technologies of sulfur trioxide according to claim 1,
It is characterized in that, step (5) heating temperature is 321-339 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229083A (en) * | 2019-06-27 | 2019-09-13 | 九江学院 | A kind of preparation method of G salt |
| CN112961034A (en) * | 2021-02-23 | 2021-06-15 | 上海东庚化工技术有限公司 | Clean production process of naphthol by taking sulfur trioxide as raw material |
| CN112979427A (en) * | 2021-02-23 | 2021-06-18 | 上海东庚化工技术有限公司 | Process for synthesizing naphthol through sulfur trioxide indirect sulfonation reaction |
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| CN112961034A (en) * | 2021-02-23 | 2021-06-15 | 上海东庚化工技术有限公司 | Clean production process of naphthol by taking sulfur trioxide as raw material |
| CN112979427A (en) * | 2021-02-23 | 2021-06-18 | 上海东庚化工技术有限公司 | Process for synthesizing naphthol through sulfur trioxide indirect sulfonation reaction |
| CN112961034B (en) * | 2021-02-23 | 2023-07-25 | 上海东庚化工技术有限公司 | Clean naphthol production process taking sulfur trioxide as raw material |
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