CN212222833U - Resorcinol neutralization reaction device - Google Patents

Resorcinol neutralization reaction device Download PDF

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CN212222833U
CN212222833U CN202020886745.3U CN202020886745U CN212222833U CN 212222833 U CN212222833 U CN 212222833U CN 202020886745 U CN202020886745 U CN 202020886745U CN 212222833 U CN212222833 U CN 212222833U
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pipeline
neutralization
neutralization reaction
sodium sulfite
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乐金波
张泉森
高天庆
高晶
何彪
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Hami Shengdian Technology Co ltd
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Hami Shengdian Technology Co ltd
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Abstract

The utility model provides a neutralization reaction device of resorcinol, including neutralization reaction cauldron, be provided with agitating unit in neutralization reaction cauldron, top at this neutralization reaction cauldron is provided with sodium sulfite solution and adds the pipeline, pipeline and sulfur dioxide tail gas collection pipeline are added to the disulfonation result, sodium sulfite solution adds the pipeline and links to each other with sodium sulfite metering tank bottom baiting valve, be provided with sodium sulfite replenishment pipeline on the sodium sulfite metering tank, neutralization reaction cauldron's bottom is provided with ejection of compact pipeline and links to each other with the circulating pump, one of them branch pipe of export pipeline of circulating pump links to each other with the material import of neutralization condenser, the material export of neutralization condenser links to each other with neutralization reaction cauldron's top feed back mouth, another branch pipe of export pipeline of circulating pump is neutralization liquid ejection of compact pipeline, all be provided with the valve on two branch pipes of the export pipeline of circulating pump. Safe, environment-friendly and suitable for industrial popularization.

Description

Resorcinol neutralization reaction device
Technical Field
The utility model relates to a neutralization reaction device of resorcinol belongs to the chemical production field.
Background
Resorcinol is a very widely used fine organic chemical raw material, and plays an extremely important role in the fields of agriculture, dyes, coatings, medicines, plastics, rubbers and electronic chemicals. In the medical field, resorcinol has a certain bactericidal effect, can treat fungal infection skin diseases or is used as an intestinal disinfectant, and is also an important medical intermediate, for example, the resorcinol is an initial raw material of an antituberculous drug p-aminosalicylic acid drug.
Currently, there are companies that can make over ten thousand tons annually internationally, the U.S. edspeek chemical company and japanese sumitomo chemistry. The consumption of resorcinol in the united states in 2004 reaches 1.6 ten thousand tons and in japan 6 kilotons, and is expected to increase at a rate of 3.5% per year. Along with the improvement of living standard of people, the domestic demand of resorcinol is continuously increased, the resorcinol price is greatly increased due to the strong demand, and the construction of resorcinol is high in China.
The domestic industrial production method of the resorcinol comprises the following steps: benzene sulfonation alkali fusion method, group substitution method, arylation method, phenol hydroxylation method and m-diisopropylbenzene oxidation method.
The benzene sulfonation alkali fusion method uses benzene as raw materialIs a starting material, has simple process condition and mature technology, is a domestic main production process at present, but has great environmental pollution. In the production process of the product, a large amount of strong acid and strong base are needed, and a large amount of inorganic salt Na is generated at the same time2S04、Na2SO3(in the traditional process, fuming sulfuric acid is used for sulfonation reaction, sodium hydroxide is used for neutralization, dilute sulfuric acid or hydrochloric acid is used for acidification, so that a large amount of sodium sulfate or sodium chloride byproducts are generated, the sodium sulfate is difficult to treat, the difficulty in treating three wastes is increased), and the environmental pressure is higher. Wherein sodium sulfate is mainly generated in the processes of sulfonation and acidification, sodium sulfite is generated in the process of alkali fusion, and the main sulfonation process is step-by-step sulfonation, such as:
the first process comprises the following steps: the initial process comprises two steps of sulfonation, wherein in the first step, fuming sulfuric acid and benzene are used for primary sulfonation at about 70 ℃, the sulfonated product is transferred to a second sulfonation kettle after the first step is completed, the fuming sulfuric acid is used for reacting at about 170 ℃ to prepare m-benzene disulfonic acid, sodium hydroxide is used for neutralizing to produce 3.8 tons of sodium sulfate generated by one ton of resorcinol, the sodium sulfate and the sodium hydroxide are used for reacting in an alkali melting kettle, and the molar ratio of the sodium hydroxide to the benzene is 5: 1, generating 3.4 tons of by-product sodium sulfite, and acidifying with sulfuric acid to generate 3.8 tons of sodium sulfate.
And a second process: the first step is to use fuming sulfuric acid to carry out primary sulfonation at about 70 ℃, the sulfonated product is transferred to a second sulfonation kettle after the first step is finished, sulfur trioxide is used to react at about 140 ℃ to prepare the m-benzene disulfonic acid, the process is improved on the first process, sodium sulfate generated by producing one ton of resorcinol after sodium hydroxide is neutralized is 1.9 ton, the sodium sulfate and the sodium hydroxide react in an alkali melting kettle, and the molar ratio of the sodium hydroxide to benzene is 5: 1, generating 3.4 tons of by-product sodium sulfite, and acidifying with sulfuric acid to generate 3.8 tons of sodium sulfate.
In view of the above problems, the applicant has devised an environmentally friendly and economical resorcinol production method. The method comprises the steps of primary sulfonation, secondary sulfonation, neutralization, alkali fusion, dilution, acidification, extraction and concentration, wherein the primary sulfonation and the secondary sulfonation are both sulfonated by sulfur trioxide, the neutralization is carried out by sodium sulfite, sulfur dioxide generated in the neutralization is used for the acidification, and the sodium sulfite generated in the alkali fusion and the acidification is used for the neutralization reaction. The production method is also a problem which needs to be solved urgently aiming at a neutralization reaction device which is reasonable in design and high in efficiency.
SUMMERY OF THE UTILITY MODEL
This in order to solve above-mentioned technical problem, the utility model provides a neutralization reaction device of resorcinol, safety, environmental protection, high efficiency.
In order to realize the above object of the utility model, the utility model provides a neutralization reaction device of resorcinol, including neutralization reaction cauldron, be provided with agitating unit, its characterized in that in the neutralization reaction cauldron: be provided with sodium sulfite solution at this neutralization reaction kettle's top and add pipeline, disulfonate result and add pipeline and sulfur dioxide tail gas collection pipeline, sodium sulfite solution adds the pipeline and links to each other with sodium sulfite metering tank bottom baiting valve, be provided with sodium sulfite additional line on the sodium sulfite metering tank, neutralization reaction kettle's bottom is provided with discharge line and links to each other with the circulating pump, one of them branch pipe of export pipeline of circulating pump links to each other with the material import of neutralization condenser, the material export of neutralization condenser links to each other with neutralization reaction kettle's top feed back mouth, and another branch pipe of export pipeline of circulating pump is neutralization liquid discharge pipeline, all be provided with the valve on two branch pipes of the export pipeline of circulating pump.
By adopting the scheme, the sodium sulfite is used for neutralizing the disulfonated product, particularly the sodium sulfite can be obtained from the subsequent acidification and alkali fusion processes, the use amount of sodium hydroxide is reduced, and the salt yield is reduced. And collecting sulfur dioxide generated by neutralization through a sulfur dioxide tail gas collecting pipeline for a subsequent acidification process. In the reaction process, the heat of production gets back to neutralization reaction cauldron after through external condenser condensation, compares than reation kettle directly with the intermediate layer condensation, and the condensation effect is better to still be favorable to the intensive mixing of material like this, improve neutralization reaction efficiency.
In the scheme, the neutralization reaction kettle is also provided with a temperature sensor. For monitoring the temperature in the neutralization reactor.
In the scheme, the method comprises the following steps: the circulating pumps are two, inlets of the two circulating pumps are connected with a discharge pipeline of the neutralization reaction kettle, outlets of the two circulating pumps are connected with an outlet main pipeline, one branch pipe of the outlet main pipeline is connected with the condenser, and the other branch pipe of the outlet main pipeline is a neutralization liquid discharge pipeline. The two circulating pumps are opened and closed.
In the scheme, the method comprises the following steps: the top of neutralization reaction cauldron is provided with two sulfur dioxide discharge ports, and these two sulfur dioxide discharge ports all link to each other with sulfur dioxide tail gas collection pipeline. Is beneficial to the removal of the sulfur dioxide of the reaction product.
Has the advantages that: the utility model discloses a neutralization reaction device can in time remove the heat that the reaction produced, guarantees going on smoothly fully of reaction, reduces the side reaction, improves the reaction yield, improves product quality. The utility model discloses each raw materials passes through the sealed joining of pipeline, reduces personnel's contact, and safety, the environmental protection is fit for the industrialization and promotes.
Drawings
Fig. 1 is a process flow diagram of the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to the following examples and drawings.
Example 1
As shown in figure 1, the utility model discloses a neutralization reaction device of resorcinol is added pipeline 3, disulfonate result by neutralization reaction kettle 1, agitating unit 2, sodium sulfite solution, and pipeline 4, sulfur dioxide tail gas collection pipeline 5, sodium sulfite metering tank 6, sodium sulfite make-up pipeline 7, circulating pump 8, neutralization liquid discharging pipeline 9, neutralization condenser 10, temperature sensor 11 and connecting line and valve are constituteed to the disulfonate result.
Neutralization reaction kettle 1 adopts general reation kettle, is provided with agitating unit 2 in neutralization reaction kettle 1, is provided with sodium sulfite solution at this neutralization reaction kettle 1's top and adds pipeline 3, the disulfonation result adds pipeline 4 and sulfur dioxide tail gas collecting line 5, and preferred neutralization reaction kettle 1's top is provided with two sulfur dioxide discharge ports, and these two sulfur dioxide discharge ports all link to each other with sulfur dioxide tail gas collecting line 5. The neutralization reaction kettle 1 is also provided with a temperature sensor 11.
Sodium sulfite solution adds pipeline 3 and links to each other with 6 bottom baiting valves of sodium sulfite metering tank, be provided with sodium sulfite replenishment pipeline 7 on the sodium sulfite metering tank 6, neutralization reaction kettle 1's bottom is provided with discharging line and links to each other with circulating pump 8, one of them branch pipe of circulating pump 8's outlet line links to each other with neutralization condenser 10's material import, neutralization condenser 10 adopts the circulating condensate water to condense, neutralization condenser 10's material export links to each other with neutralization reaction kettle 1's top feed back mouth, another branch pipe of circulating pump 8's outlet line is neutralization liquid discharging line 9, all be provided with the valve on two branch pipes of circulating pump 8's outlet line. Preferably, two circulating pumps 8 are provided, the inlets of the two circulating pumps 8 are connected with the discharge pipeline of the neutralization reaction kettle 1, the outlets of the two circulating pumps 8 are connected with the outlet main pipeline, one branch pipe of the outlet main pipeline is connected with the condenser 10, and the other branch pipe is the neutralization liquid discharge pipeline 9. The neutralizing liquid discharging pipeline 9 is connected with a neutralizing liquid metering tank (not shown in the figure), and the top of the neutralizing liquid metering tank is provided with a tail gas collecting pipeline.
The above description is provided for the purpose of describing the present invention in more detail with reference to the preferred embodiments, and it should not be construed that the present invention is limited to these descriptions, and it will be apparent to those skilled in the art that the present invention can be implemented in many ways without departing from the spirit and scope of the present invention.

Claims (4)

1. The utility model provides a neutralization reaction device of resorcinol, includes neutralization reaction cauldron, be provided with agitating unit in the neutralization reaction cauldron, its characterized in that: be provided with sodium sulfite solution at this neutralization reaction kettle's top and add pipeline, disulfonate result and add pipeline and sulfur dioxide tail gas collection pipeline, sodium sulfite solution adds the pipeline and links to each other with sodium sulfite metering tank bottom baiting valve, be provided with sodium sulfite additional line on the sodium sulfite metering tank, neutralization reaction kettle's bottom is provided with discharge line and links to each other with the circulating pump, one of them branch pipe of export pipeline of circulating pump links to each other with the material import of neutralization condenser, the material export of neutralization condenser links to each other with neutralization reaction kettle's top feed back mouth, and another branch pipe of export pipeline of circulating pump is neutralization liquid discharge pipeline, all be provided with the valve on two branch pipes of the export pipeline of circulating pump.
2. The apparatus for neutralization of resorcinol according to claim 1, wherein: and the neutralization reaction kettle is also provided with a temperature sensor.
3. The apparatus for neutralization reaction of resorcinol according to claim 1 or 2, wherein: the circulating pumps are two, inlets of the two circulating pumps are connected with a discharge pipeline of the neutralization reaction kettle, outlets of the two circulating pumps are connected with an outlet main pipeline, one branch pipe of the outlet main pipeline is connected with the condenser, and the other branch pipe of the outlet main pipeline is a neutralization liquid discharge pipeline.
4. The apparatus for neutralization of resorcinol according to claim 3, wherein: the top of neutralization reaction cauldron is provided with two sulfur dioxide discharge ports, and these two sulfur dioxide discharge ports all link to each other with sulfur dioxide tail gas collection pipeline.
CN202020886745.3U 2020-05-25 2020-05-25 Resorcinol neutralization reaction device Active CN212222833U (en)

Priority Applications (1)

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CN202020886745.3U CN212222833U (en) 2020-05-25 2020-05-25 Resorcinol neutralization reaction device

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Application Number Priority Date Filing Date Title
CN202020886745.3U CN212222833U (en) 2020-05-25 2020-05-25 Resorcinol neutralization reaction device

Publications (1)

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CN212222833U true CN212222833U (en) 2020-12-25

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