阅读说明：本技术 一种新型工作液制双氧水的制备工艺 (Preparation process for preparing hydrogen peroxide from novel working solution ) 是由 夏旭东 蔡荣成 唐旻富 于 2020-07-23 设计创作，主要内容包括：本发明公开了一种新型工作液制双氧水的制备工艺,包括以下步骤：步骤一,制液；步骤二,氢化；步骤三,氧化；步骤四,萃取；步骤五,净化；步骤六,再生；其中在上述步骤一中,取适量的四丁基脲和芳烃溶剂油按25：75的比例注入配制釜中,再用气泵注入蒸汽,升温后进行一次搅拌；本发明用四丁基脲取代了磷酸三辛酯,从而提高了氢蒽醌的溶解度,增大了过氧化氢在两相中的分配系数、与水密度差和表面张力,降低了萃取的难度,提高了氢化和萃取的效率,减少了工作液的循环量,节省了工作液的的再生成本,有利于双氧水的大批量生产,通过向净化塔中注入芳烃,从而将尾液中残存的降解物与双氧水原液分离开,提高了净化的效率,保障了双氧水成品的纯度。(The invention discloses a preparation process for preparing hydrogen peroxide from novel working solution, which comprises the following steps: step one, preparing liquid; step two, hydrogenation; step three, oxidizing; step four, extraction; step five, purifying; step six, regeneration; in the first step, taking a proper amount of tetrabutyl urea and aromatic hydrocarbon solvent oil, and mixing the components in a ratio of 25: 75, injecting the mixture into a preparation kettle, injecting steam by using an air pump, and stirring for the first time after heating; the invention replaces trioctyl phosphate with tetrabutyl urea, thereby improving the solubility of anthraquinone, increasing the distribution coefficient of hydrogen peroxide in two phases, the difference of water density and surface tension, reducing the extraction difficulty, improving the efficiency of hydrogenation and extraction, reducing the circulation amount of working liquid, saving the regeneration cost of the working liquid, being beneficial to the mass production of hydrogen peroxide, separating the residual degradation product in tail liquid from the hydrogen peroxide stock solution by injecting aromatic hydrocarbon into the purification tower, improving the purification efficiency and ensuring the purity of the hydrogen peroxide finished product.)

1. A novel preparation process for preparing hydrogen peroxide from working solution comprises the following steps: step one, preparing liquid; step two, hydrogenation; step three, oxidizing; step four, extraction; step five, purifying; step six, regeneration; the method is characterized in that:

in the first step, taking a proper amount of tetrabutyl urea and aromatic hydrocarbon solvent oil, and mixing the components in a ratio of 25: 75, injecting the mixture into a preparation kettle, injecting steam by using an air pump, heating, stirring for the first time, taking proper amounts of dimethyl anthraquinone and tetrahydro dimethyl anthraquinone, mixing the mixture according to a ratio of 60: 40, preparing the working solution into a working solution after secondary stirring, and feeding the working solution into a liquid storage tank;

in the second step, the working solution prepared in the first step is taken out from a liquid storage tank, the working solution is conveyed into a hydrogenation tower after being treated by a filter and a preheater, compressed hydrogen is injected by an air compressor, the working solution is hydrogenated by matching with a palladium catalyst bed in the hydrogenation tower, so that dimethylanthraquinone is converted into dimethylanthraquinone, tetrahydrodimethylanthraquinone is converted into tetrahydrodimethylanthraquinone, the mixture is conveyed into a gas-liquid separator, tail gas and hydrogenated liquid are separated, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank after the tail gas is treated by a condenser, residual waste gas is discharged, and finally the hydrogenated liquid enters a hydrogenated liquid storage tank after being treated by the filter, a heat exchanger and a hydrogenated white soil bed;

in the third step, the hydrogenated liquid prepared in the second step is taken out from a hydrogenated liquid storage tank, the hydrogenated liquid is treated by a cooler and then is conveyed into an oxidation tower, compressed oxygen is injected by an air compressor to oxidize the hydrogenated liquid, so that the dimethyl hydroanthraquinone is converted into dimethyl anthraquinone, the tetrahydro dimethyl hydroanthraquinone is converted into tetrahydro dimethyl anthraquinone, hydrogen peroxide is generated, the mixture is conveyed into a gas-liquid separator, tail gas and oxidation liquid are separated, the tail gas is treated by a condenser, a buffer tank, an adsorption tank and a bubble column, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally the oxidation liquid enters an oxidation liquid storage tank after being treated by a filter, a heat exchanger and an oxidation clay bed;

in the fourth step, the oxidation liquid prepared in the third step is taken out from the oxidation liquid storage tank, the oxidation liquid is treated by a cooler and then is conveyed into an extraction tower, pure water is injected by a water pump to extract the oxidation liquid, hydrogen peroxide which is easy to dissolve in water is converted into hydrogen peroxide, then the mixture is conveyed into a coalescence separator, raffinate and hydrogen peroxide extract are separated out, the raffinate enters the raffinate storage tank, and finally the hydrogen peroxide extract enters the extract storage tank after being treated by a heat exchanger;

in the fifth step, firstly, the hydrogen peroxide extract prepared in the fourth step is taken out of the extract storage tank and conveyed to a purification tower, then aromatic hydrocarbon is injected by a water pump, the hydrogen peroxide extract is purified into a hydrogen peroxide stock solution with the concentration of 27.5-35%, then the mixture is conveyed to a thin product separator, tail liquid and the hydrogen peroxide stock solution are separated, the aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally the hydrogen peroxide stock solution is treated by a heat exchanger and then enters a finished product tank to finish primary production;

and in the sixth step, the raffinate separated in the fourth step is taken out from a raffinate storage tank, conveyed to a drying tower, injected with a potassium carbonate solution by a water pump to decompose hydrogen peroxide remaining in the raffinate, conveyed to an alkali-liquid separator to remove water in the extract, and finally conveyed to a regenerated clay bed to be subjected to dehydrogenation treatment by active alumina to convert dimethyl hydroanthraquinone remaining in the extract into dimethyl anthraquinone and tetrahydro dimethyl hydroanthraquinone into tetrahydro dimethyl anthraquinone, so that the extract is regenerated into a working solution and recycled to a liquid storage tank to enter the next cycle.

2. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the first step, the preparation temperature of the preparation kettle is 45-55 ℃, the stirring time is 50-110 min, and the stirring speed is 5-10 r/s.

3. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the second step, the operation pressure of the hydrogenation tower is 0.20-0.30 MPa, and the hydrogenation temperature is 55-75 ℃.

4. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the second step, the outlet temperature of the preheater is 30-50 ℃, the outlet temperature of the condenser is 10-30 ℃, and the outlet temperature of the heat exchanger is 40-50 ℃.

5. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the third step, the operating pressure of the oxidation tower is 0.25-0.35 MPa, and the oxidation temperature is 40-50 ℃.

6. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the third step, the outlet temperature of the cooler is 30-40 ℃, and the outlet temperature of the condenser is 10-30 ℃.

7. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the fourth step, the operating pressure of the extraction tower is normal pressure, the extraction temperature is 35-55 ℃, and the extraction ratio of the oxidizing liquid to the pure water is 1: 30-1: 60.

8. the preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the fourth step, the outlet temperature of the cooler is 10-30 ℃, and the outlet temperature of the heat exchanger is 30-35 ℃.

9. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the fifth step, the operation pressure of the purification tower is normal pressure, and the purification temperature is 35-40 ℃.

10. The preparation process for preparing hydrogen peroxide from novel working solution according to claim 1, which is characterized by comprising the following steps: in the sixth step, the operation pressure of the drying tower is normal pressure, and the drying temperature is 35-45 ℃.

Technical Field

The invention relates to the technical field of hydrogen peroxide production, in particular to a novel preparation process for preparing hydrogen peroxide from working solution.

Background

Hydrogen peroxide, a known hydrogen peroxide aqueous solution, generally refers to a colorless transparent aqueous solution generated by mixing hydrogen peroxide and water, is a strong oxidant, and is widely applied to the fields of industrial bleaching, food sterilization, surgical disinfection and the like.

However, in the conventional hydrogen peroxide preparation process, the working solution mostly uses trioctyl phosphate as a solvent of hydroanthraquinone, and has low solubility, small distribution coefficient of hydrogen peroxide in two phases, insufficient surface tension and small difference with water density, so that the hydrogenation and extraction efficiency is reduced, the circulation amount of the working solution is increased, the regeneration cost is increased, and the large-scale production of hydrogen peroxide is not facilitated.

Disclosure of Invention

The invention aims to provide a novel preparation process for preparing hydrogen peroxide from working solution, which aims to solve the problems in the background art.

In order to solve the technical problems, the invention provides the following technical scheme: a novel preparation process for preparing hydrogen peroxide from working solution comprises the following steps: step one, preparing liquid; step two, hydrogenation; step three, oxidizing; step four, extraction; step five, purifying; step six, regeneration;

in the first step, taking a proper amount of tetrabutyl urea and aromatic hydrocarbon solvent oil, and mixing the components in a ratio of 25: 75, injecting the mixture into a preparation kettle, injecting steam by using an air pump, heating, stirring for the first time, taking proper amounts of dimethyl anthraquinone and tetrahydro dimethyl anthraquinone, mixing the mixture according to a ratio of 60: 40, preparing the working solution into a working solution after secondary stirring, and feeding the working solution into a liquid storage tank;

in the second step, the working solution prepared in the first step is taken out from a liquid storage tank, the working solution is conveyed into a hydrogenation tower after being treated by a filter and a preheater, compressed hydrogen is injected by an air compressor, the working solution is hydrogenated by matching with a palladium catalyst bed in the hydrogenation tower, so that dimethylanthraquinone is converted into dimethylanthraquinone, tetrahydrodimethylanthraquinone is converted into tetrahydrodimethylanthraquinone, the mixture is conveyed into a gas-liquid separator, tail gas and hydrogenated liquid are separated, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank after the tail gas is treated by a condenser, residual waste gas is discharged, and finally the hydrogenated liquid enters a hydrogenated liquid storage tank after being treated by the filter, a heat exchanger and a hydrogenated white soil bed;

in the third step, the hydrogenated liquid prepared in the second step is taken out from a hydrogenated liquid storage tank, the hydrogenated liquid is treated by a cooler and then is conveyed into an oxidation tower, compressed oxygen is injected by an air compressor to oxidize the hydrogenated liquid, so that the dimethyl hydroanthraquinone is converted into dimethyl anthraquinone, the tetrahydro dimethyl hydroanthraquinone is converted into tetrahydro dimethyl anthraquinone, hydrogen peroxide is generated, the mixture is conveyed into a gas-liquid separator, tail gas and oxidation liquid are separated, the tail gas is treated by a condenser, a buffer tank, an adsorption tank and a bubble column, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally the oxidation liquid enters an oxidation liquid storage tank after being treated by a filter, a heat exchanger and an oxidation clay bed;

in the fourth step, the oxidation liquid prepared in the third step is taken out from the oxidation liquid storage tank, the oxidation liquid is treated by a cooler and then is conveyed into an extraction tower, pure water is injected by a water pump to extract the oxidation liquid, hydrogen peroxide which is easy to dissolve in water is converted into hydrogen peroxide, then the mixture is conveyed into a coalescence separator, raffinate and hydrogen peroxide extract are separated out, the raffinate enters the raffinate storage tank, and finally the hydrogen peroxide extract enters the extract storage tank after being treated by a heat exchanger;

in the fifth step, firstly, the hydrogen peroxide extract prepared in the fourth step is taken out of the extract storage tank and conveyed to a purification tower, then aromatic hydrocarbon is injected by a water pump, the hydrogen peroxide extract is purified into a hydrogen peroxide stock solution with the concentration of 27.5-35%, then the mixture is conveyed to a thin product separator, tail liquid and the hydrogen peroxide stock solution are separated, the aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally the hydrogen peroxide stock solution is treated by a heat exchanger and then enters a finished product tank to finish primary production;

and in the sixth step, the raffinate separated in the fourth step is taken out from a raffinate storage tank, conveyed to a drying tower, injected with a potassium carbonate solution by a water pump to decompose hydrogen peroxide remaining in the raffinate, conveyed to an alkali-liquid separator to remove water in the extract, and finally conveyed to a regenerated clay bed to be subjected to dehydrogenation treatment by active alumina to convert dimethyl hydroanthraquinone remaining in the extract into dimethyl anthraquinone and tetrahydro dimethyl hydroanthraquinone into tetrahydro dimethyl anthraquinone, so that the extract is regenerated into a working solution and recycled to a liquid storage tank to enter the next cycle.

According to the technical scheme, in the first step, the preparation temperature of the preparation kettle is 45-55 ℃, the stirring time is 50-110 min, and the stirring speed is 5-10 r/s.

According to the technical scheme, in the second step, the operation pressure of the hydrogenation tower is 0.20-0.30 MPa, and the hydrogenation temperature is 55-75 ℃.

According to the technical scheme, in the second step, the outlet temperature of the preheater is 30-50 ℃, the outlet temperature of the condenser is 10-30 ℃, and the outlet temperature of the heat exchanger is 40-50 ℃.

According to the technical scheme, in the third step, the operating pressure of the oxidation tower is 0.25-0.35 MPa, and the oxidation temperature is 40-50 ℃.

According to the technical scheme, in the third step, the outlet temperature of the cooler is 30-40 ℃, and the outlet temperature of the condenser is 10-30 ℃.

According to the technical scheme, in the fourth step, the operating pressure of the extraction tower is normal pressure, the extraction temperature is 35-55 ℃, and the extraction ratio of the oxidizing liquid to pure water is 1: 30-1: 60.

according to the technical scheme, in the fourth step, the outlet temperature of the cooler is 10-30 ℃, and the outlet temperature of the heat exchanger is 30-35 ℃.

According to the technical scheme, in the fifth step, the operation pressure of the purification tower is normal pressure, and the purification temperature is 35-40 ℃.

According to the technical scheme, in the sixth step, the operation pressure of the drying tower is normal pressure, and the drying temperature is 35-45 ℃.

Compared with the prior art, the invention has the following beneficial effects: the novel preparation process for preparing hydrogen peroxide by using the working solution adopts tetrabutyl urea as a solvent of hydroanthraquinone to replace the traditional trioctyl phosphate, thereby improving the solubility of hydroanthraquinone, increasing the distribution coefficient of hydrogen peroxide in two phases, the difference between the distribution coefficient and water density and the surface tension, reducing the extraction difficulty, improving the hydrogenation and extraction efficiency, reducing the circulation volume of the working solution, saving the regeneration cost of the working solution and being beneficial to the mass production of the hydrogen peroxide; in the purification step, aromatic hydrocarbon is injected into the purification tower, so that the separation of the residual degradation products in the hydrogen peroxide stock solution and the tail solution is facilitated, and the purification efficiency and the purity of the hydrogen peroxide finished product are improved.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1, the present invention provides a technical solution: a novel preparation process for preparing hydrogen peroxide from working solution comprises the following steps: step one, preparing liquid; step two, hydrogenation; step three, oxidizing; step four, extraction; step five, purifying; step six, regeneration;

in the first step, taking a proper amount of tetrabutyl urea and aromatic hydrocarbon solvent oil, and mixing the components in a ratio of 25: 75, injecting the mixture into a preparation kettle, injecting steam by using an air pump, heating, stirring for the first time, taking proper amounts of dimethyl anthraquinone and tetrahydro dimethyl anthraquinone, mixing the mixture according to a ratio of 60: 40, preparing the working solution into a liquid storage tank after secondary stirring, wherein the preparation temperature of the preparation kettle is 45-55 ℃, the stirring time is 50-110 min, and the stirring speed is 5-10 r/s;

in the second step, the working solution prepared in the first step is taken out from a liquid storage tank, the working solution is processed by a filter and a preheater and then is conveyed into a hydrogenation tower, the outlet temperature of the preheater is 30-50 ℃, the operating pressure of the hydrogenation tower is 0.20-0.30 MPa, the hydrogenation temperature is 55-75 ℃, compressed hydrogen is injected by an air compressor, the working solution is hydrogenated by matching with a palladium catalyst bed in the hydrogenation tower, so that the dimethylanthraquinone is converted into the dimethylanthraquinone and the tetrahydrodimethylanthraquinone is converted into the tetrahydrodimethylanthraquinone, then the mixture is conveyed into a gas-liquid separator, tail gas and hydrogenated liquid are separated, the aromatic hydrocarbon enters a waste aromatic hydrocarbon tank after the tail gas is processed by a condenser, residual waste gas is discharged, the outlet temperature of the condenser is 10-30 ℃, and finally the hydrogenated liquid enters a hydrogenated liquid storage tank after the hydrogenated liquid is processed by the filter, a heat exchanger and, the outlet temperature of the heat exchanger is 40-50 ℃;

wherein in the third step, the hydrogenation liquid prepared in the second step is taken out from the hydrogenation liquid storage tank, treated by a cooler and then conveyed to an oxidation tower, the outlet temperature of the cooler is 30-40 ℃, the operating pressure of the oxidation tower is 0.25-0.35 MPa, the oxidation temperature is 40-50 ℃, compressed oxygen is injected by an air compressor, oxidizing the hydrogenated liquid to convert dimethyl hydroanthraquinone into dimethyl anthraquinone and tetrahydro dimethyl hydroanthraquinone into tetrahydro dimethyl anthraquinone and produce hydrogen peroxide, then the mixture is conveyed into a gas-liquid separator to separate out tail gas and oxidation liquid, the tail gas is treated by a condenser, a buffer tank, an adsorption tank and a bubble column, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally oxidizing liquid enters an oxidizing liquid storage tank after being treated by a filter, a heat exchanger and an oxidized clay bed, wherein the outlet temperature of a condenser is 10-30 ℃;

in the fourth step, the oxidation liquid prepared in the third step is taken out of the oxidation liquid storage tank, treated by a cooler and then conveyed into an extraction tower, the outlet temperature of the cooler is 10-30 ℃, the operating pressure of the extraction tower is normal pressure, the extraction temperature is 35-55 ℃, and the extraction ratio of the oxidation liquid to pure water is 1: 30-1: injecting pure water by using a water pump, extracting the oxidation liquid to convert hydrogen peroxide which is easy to dissolve in water into hydrogen peroxide, conveying the mixture into a coalescence separator, separating out raffinate and hydrogen peroxide extract, introducing the raffinate into a raffinate storage tank, and finally introducing the hydrogen peroxide extract into an extract storage tank after being treated by a heat exchanger, wherein the outlet temperature of the heat exchanger is 30-35 ℃;

in the fifth step, firstly, the hydrogen peroxide extract prepared in the fourth step is taken out of an extract storage tank and conveyed into a purification tower, the operating pressure of the purification tower is normal pressure, the purification temperature is 35-40 ℃, aromatic hydrocarbon is injected by a water pump, the hydrogen peroxide extract is purified into hydrogen peroxide stock solution with the concentration of 27.5-35%, then the mixture is conveyed into a thin product separator, tail solution and hydrogen peroxide stock solution are separated, aromatic hydrocarbon enters a waste aromatic hydrocarbon tank, residual waste gas is discharged, and finally the hydrogen peroxide stock solution enters a finished product tank after being treated by a heat exchanger to finish primary production;

and in the sixth step, the raffinate separated in the fourth step is taken out of a raffinate storage tank and conveyed into a drying tower, the operating pressure of the drying tower is normal pressure, the drying temperature is 35-45 ℃, a potassium carbonate solution is injected by a water pump to decompose hydrogen peroxide remaining in the raffinate, the mixture is conveyed into an alkali-liquid separator to remove water in the extract, and finally the extract is conveyed into a regenerated clay bed and subjected to dehydrogenation treatment by activated alumina to convert dimethyl hydroanthraquinone remaining in the extract into dimethyl anthraquinone and tetrahydro dimethyl hydroanthraquinone into tetrahydro dimethyl anthraquinone, so that the extract is regenerated into a working solution and is recycled into a liquid storage tank to enter the next cycle.

Based on the above, the invention has the advantages that the tetrabutyl urea is used for replacing trioctyl phosphate, so that the solubility of the hydroanthraquinone is improved, the distribution coefficient of the hydrogen peroxide in two phases, the water density difference and the surface tension of the hydrogen peroxide are increased, the extraction difficulty is reduced, the hydrogenation and extraction efficiency is improved, the circulation amount of the working solution is reduced, the regeneration cost of the working solution is saved, the mass production of the hydrogen peroxide is facilitated, and the residual degradation product in the tail solution is separated from the hydrogen peroxide stock solution by injecting the aromatic hydrocarbon into the purification tower, so that the purification efficiency is improved, and the purity of the hydrogen peroxide finished product is ensured.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.