CN1074895A - Processes and apparatus with producing phenol by acidifying method with sulfur - Google Patents
Processes and apparatus with producing phenol by acidifying method with sulfur Download PDFInfo
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- CN1074895A CN1074895A CN 92100510 CN92100510A CN1074895A CN 1074895 A CN1074895 A CN 1074895A CN 92100510 CN92100510 CN 92100510 CN 92100510 A CN92100510 A CN 92100510A CN 1074895 A CN1074895 A CN 1074895A
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Abstract
A kind of improved, turn to the Processes and apparatus of the production phenol of characteristics with thiosulfonic acid.Its sulfur dioxide gas by generating with sulfur burning replaces dilute sulphuric acid acidifying sodium phenylate, thereby produces phenol.Improved technology has solved waste water pollution problem.Its acidizing unit is simple in structure, is convenient to make and operation, and the ratio of first-grade products of phenol reaches 100%.
Description
The present invention relates to a kind of improved phenol production Processes and apparatus, particularly carry out industrial Processes and apparatus, belong to organic chemical industry's preparing technical field with sulfonated alkali fusion method.
Phenol is the important basic organic synthesis raw material of chemical industry, and it is widely used in plastics, medicine, agricultural chemicals, synthesising fibre and petrochemical industry etc.Twentieth century is because the growing Pyrogentisinic Acid's of resol demand surge stimulates the method that has produced many synthesizing phenols, as benzene process for oxychlorination, hexanaphthene method, benzene direct oxidation method, toluene oxidation method, cumene method, sulfonated alkali fusion method or the like.Advantages such as wherein, sulfonated alkali fusion method is low with its raw material consumption quota, and good product quality and technology are reliable and still being adopted by many producers.But, in the technology that adopts traditional sulfonated alkali fusion method production phenol, after alkali fusion procedure is finished, need enter acidizing process and carry out acidifying, traditional acidifying be with in the Phenylsulfonic acid and after the product sulfurous gas of paying be the acidifying raw material, because in self and the dioxide production deficiency in the operation, still have the sodium phenylate about 15% to come balanced production with the dilute sulphuric acid acidifying, its reaction formula is as follows:
Wherein, resultant sodium sulfate is useless waste material in phenol production technology.And one ton of phenol of every production discharges 1% phenolic wastewater 3-5 ton approximately, and sewage load is big, and producer need invest 1,000,000 yuan in addition and be handled, and nonetheless, its effect is still not satisfactory.
The purpose of this invention is to provide a kind of improved sulfonated alkali fusion method and produce the novel process of phenol, this technology should have and not arrange or do not arrange substantially process spent water, and the raw material sources that participate in reaction are easy to get, stable reaction safety, the advantage that cost is suitable.
The objective of the invention is by producing sulfur dioxide gas, replace dilute sulphuric acid acidifying sodium phenylate to realize with sulfur burning.
The invention will be further described below with reference to traditional sulfonated alkali fusion method.
Fig. 1 is a sulfur acidification equipment structural representation of the present invention.
Fig. 2 is the sectional view of sulfurous gas producer.
The technical process that the tradition sulfonated alkali fusion method is produced phenol is: sulfonation → neutralization → alkali fusion → acidifying → crude phenol neutralization → distillation → finished product.
Wherein, the effect of each operation and reaction formula are: sulfonation, its effect are that benzene feedstock and sulfuric acid are carried out gas phase xanthation and obtained Phenylsulfonic acid, the principal reaction formula:
Neutralization: its effect is that the principal reaction formula is with in Phenylsulfonic acid and the sodium sulfite aqueous solution and generation benzene sulfonic acid sodium salt and sulfur dioxide gas:
Alkali fusion: its effect is that the sodium hydroxide with benzene sulfonic acid sodium salt solution and molten state acts under 300-350 ℃ of temperature and generates sodium phenylate, S-WAT and water.
Acidifying: its effect is that the sodium phenylate acidifying is become crude phenol and S-WAT.
Because of the sulfur dioxide gas scale of construction is few, need adds dilute sulphuric acid in addition and come balanced production:
The crude phenol neutralization: its effect is that the objectionable impurities sodium bisulfite in the crude phenol is neutralized with yellow soda ash.Its reaction formula is:
Distillation: the crude phenol after the neutralization carries out reduced pressure distillation through clarifying treatment, promptly obtains finished product phenol.
Sulfonated alkali fusion method after the improvement all adopts sulfur dioxide gas to come the acidifying sodium phenylate, does not come balanced production and do not re-use the dilute sulphuric acid acidifying.
Need the sulfur dioxide gas of usefulness in the reaction, can directly buy the commodity liquid sulfur dioxide, but do like this, phenol ton cost will be increased.
The present invention adopts sulfur burning to generate sulfur dioxide gas, uses sulfurous gas disacidify sodium phenylate again.Its reaction formula is:
Acidifying is carried out in the acidifying groove, sulfur dioxide gas except that by in and operation attracts, all the other are supplied by sulfur acidification equipment.When reaction mass is neutral or little acid, be the acidifying terminal point.
Adopt SO 2 acidifying, its resultant S-WAT just in time to can be used as in the Phenylsulfonic acid and operation in reaction mass.Wastewater flow rate after reaction ends seldom, one ton of phenol of every production only has 0.5 ton waste water.Except that containing crude phenol, also have remaining S-WAT still can reclaim raw material, thereby can reach closed cycle, no longer waste discharge in these waste water as phenol production.
The equipment of producing each operation use of phenol mainly comprises sulfonation equipment, neutralizing device, alkali fusion equipment, acidizing unit, crude phenol neutralizing device and distillation equipment etc., after the present invention changes acidizing process, its acidizing unit also changes thereupon, and miscellaneous equipment is constant substantially.Acidizing unit after the improvement by sulfur dioxide gas producer 1, acidification reactor 5, storage tank 4, and carry the blower fan 2 and the corrosion protection pump 3 of relevant raw material to be formed.Wherein, introduced in the storage tank 4 by pipe 6 by the sodium phenylate that alkali fusion procedure produces, fill distillation phenol water in groove, sodium phenylate is prepared burden at this.Sodium phenylate after the batching directly manages 7, corrosion protection pump 3 and manage 9 and enter reactor 5.The air outlet of carbide feed generator 1 takes over 11, is connected on the reactor 5 behind blower fan 2 and pipe 12, like this, by the sulfurous gas that carbide feed generator produces, is just sent in the reactor by blower fan, with the sodium phenylate generation acidification reaction under overhead stream.After the acidifying, generate crude phenol, reenter in the storage tank 4.
Carbide feed generator is an airtight container, is provided with some dog-houses 14 above, and sulphur is mouthful feeding since then, and required oxygen also from flowing into, promptly produces sulfurous gas here after the burning.The burning of sulphur is a thermopositive reaction, and reacted sulfur dioxide gas temperature reaches more than 200 degree, need be reduced to about the 40-50 degree.The present invention is with a water cooler 13 on pipe 11.Described water cooler is actually a closed container that is wrapped on the pipe 11, and water coolant flows to from an end, flows out from the other end.Promptly be reduced to suitable temperature behind the heat transferred water coolant of sulfur dioxide gas.
In acidization,, need to regulate the flow that adds the sodium phenylate in the reactor for dominant discharge or speed of response, for this reason, connect a return line 8, in its pipe, respectively be provided with a valve 17 at pipe 9 with between managing 6, the opening degree of variable valve, the i.e. size of may command quantity of reflux.
Also be connected to a pipe 10 on pipe 9, its effect is that the crude phenol that reaction ends is imported next process.
Also be connected to an offgas duct 21 on the top of reactor, offgas duct extend in the distillation phenol water of storage tank, and its effect is that remaining sulfur dioxide gas is imported in the phenol water again, to carry out secondary reaction.
The embodiment of an acidizing device is shown among Fig. 1, and storage tank 4 adopts cast iron or steel plate manufacturing, and corrosion protection pump adopts the glass lined corrosion protection pump of inwall, for delayed response speed, has filled some corrosion resistant fillers etc. in reactor; The sulfur dioxide gas producer welds with steel plate, and dog-house can be provided with 3; Valve 16,18,19,20 etc. is set in piping, is used to control the flow direction of reactant or resultant; For the transpiration of toxic gas, storage tank loam cake closed cover 15, and with evacuated tube 21 residual gas is directed at proper site simultaneously.
Produce phenol by Processes and apparatus provided by the invention, can satisfy the requirement of phenol production, particularly acidizing process fully, waste discharge no longer in the production.Phenol cost and equal substantially with dilute sulphuric acid acidifying phenol cost, final product quality obviously improves, and the high-grade-goods rate of phenol reaches 100%.Simultaneously, it is simple for process, is convenient to operation, and raw material is easy to get.Improved device structure is simple, is suitable for manufacturing, so very easy to utilize.
Claims (4)
1, a kind of improved technology with producing phenol by acidifying method with sulfur, it is raw material with benzene, through the sulfuric acid sulfonation operation, in the S-WAT and operation, sodium hydroxide alkali fusion operation, acidizing process, in the crude phenol and operation and distillation process, produce finished product phenol, it is characterized in that, acidizing process all adopts sulfur dioxide gas and sodium phenylate to react and generates crude phenol and S-WAT.
2, a kind of equipment with producing phenol by acidifying method with sulfur, it is by sulfonation equipment, neutralizing device, alkali fusion equipment, acidizing unit, compositions such as crude phenol neutralizing device and distillation equipment, it is characterized in that, acidizing unit is by sulfur dioxide gas producer 1, acidification reactor 5, storage tank 4 and carry the blower fan 2 of relevant raw material and corrosion protection pump 3 to form, wherein, introduce in the storage tank 4 by pipe 6 by the sodium phenylate that alkali fusion procedure produces, prepare burden with the distillation phenol water in the groove, through managing 7, corrosion protection pump 3 and pipe 9 enter reactor 5, the sulfurous gas that carbide feed generator 1 produces is through managing 11,12 and blower fan 2 send in the reactor 5, carry out acidification reaction at this and sodium phenylate, the crude phenol after the acidifying is delivered to next procedure by pipe 10.
3, equipment according to claim 2 is characterized in that, at pipe 6 with between managing 9 a return water pipe 8 is installed.
4, according to claim 2 or 3 described equipment, it is characterized in that, be with a water cooler 13 in the outside of pipe 11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92100510 CN1074895A (en) | 1992-01-30 | 1992-01-30 | Processes and apparatus with producing phenol by acidifying method with sulfur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92100510 CN1074895A (en) | 1992-01-30 | 1992-01-30 | Processes and apparatus with producing phenol by acidifying method with sulfur |
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| Publication Number | Publication Date |
|---|---|
| CN1074895A true CN1074895A (en) | 1993-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92100510 Pending CN1074895A (en) | 1992-01-30 | 1992-01-30 | Processes and apparatus with producing phenol by acidifying method with sulfur |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067674C (en) * | 1998-05-29 | 2001-06-27 | 锦洲石化天元集团公司 | Synthesis of p-cresol by direct alkali fusion method from toluene-p-sulfonic acid |
| CN108727162A (en) * | 2018-06-25 | 2018-11-02 | 宁夏金海新科化工有限公司 | The method for producing cresols based on special sulfur dioxide device |
| CN111362780A (en) * | 2020-04-21 | 2020-07-03 | 哈密盛典科技有限公司 | Method for producing resorcinol by using sulfur trioxide |
-
1992
- 1992-01-30 CN CN 92100510 patent/CN1074895A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067674C (en) * | 1998-05-29 | 2001-06-27 | 锦洲石化天元集团公司 | Synthesis of p-cresol by direct alkali fusion method from toluene-p-sulfonic acid |
| CN108727162A (en) * | 2018-06-25 | 2018-11-02 | 宁夏金海新科化工有限公司 | The method for producing cresols based on special sulfur dioxide device |
| CN108727162B (en) * | 2018-06-25 | 2021-07-23 | 宁夏金海新科化工有限公司 | Method for producing cresol based on special sulfur dioxide device |
| CN111362780A (en) * | 2020-04-21 | 2020-07-03 | 哈密盛典科技有限公司 | Method for producing resorcinol by using sulfur trioxide |
| CN111362780B (en) * | 2020-04-21 | 2022-12-27 | 哈密盛典科技有限公司 | Method for producing resorcinol by using sulfur trioxide |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |