阅读说明：本技术 有效转化并降低邻苯二甲酸二丁酯废水含氮量的设备系统 (Equipment system for effectively converting and reducing nitrogen content of dibutyl phthalate wastewater ) 是由 冯烈 金波 陈云斌 孙琪 陈慧珍 蒋开炎 于 2020-06-22 设计创作，主要内容包括：本发明涉及增塑剂制备技术领域,针对现有技术的制备增塑剂邻苯二甲酸二丁酯的排放废水中废水总氮高的问题,公开了一种降低增塑剂邻苯二甲酸二丁酯废水总氮的设备,包括废水槽,水解釜、精馏塔、冷凝器及汽液分离器,所述废水槽底端和水解釜顶端之间连通并设有废水泵,所述精馏塔下端分别与水解釜顶端和水解釜下端连通,所述精馏塔上端依次连接有冷凝器和汽液分离器,并形成闭合回路,所述汽液分离器上还设有氨吸收器,所述氨吸收器中填充有高效吸附剂,用于纯化气液分离器中分离出来的氨气。本发明通过设备在邻苯二甲酸二丁酯废水加无机强碱,水解邻苯二甲酰亚胺,降低总氮的同时,回收氨气,实现邻苯二甲酸二丁酯的环保生产。(The invention relates to the technical field of plasticizer preparation, and discloses equipment for reducing total nitrogen of plasticizer dibutyl phthalate wastewater aiming at the problem of high total nitrogen of wastewater in wastewater discharged by plasticizer dibutyl phthalate preparation in the prior art. According to the invention, the equipment is used for hydrolyzing phthalimide by adding inorganic strong base into the dibutyl phthalate wastewater, so that ammonia gas is recovered while total nitrogen is reduced, and environment-friendly production of dibutyl phthalate is realized.)

1. The equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater is characterized by comprising a wastewater tank (1), a hydrolysis kettle (3), a rectifying tower (5), a condenser (6) and a vapor-liquid separator (7), wherein a wastewater pump (2) is arranged between the bottom end of the wastewater tank (1) and the top end of the hydrolysis kettle (3), the lower end of the rectifying tower (5) is communicated with the top end of the hydrolysis kettle (3) and the lower end of the hydrolysis kettle (3) respectively, the condenser (6) and the vapor-liquid separator (7) are sequentially connected to the upper end of the rectifying tower (5) to form a closed loop, an ammonia absorber (8) is arranged on the vapor-liquid separator (7), and a high-efficiency adsorbent is filled in the ammonia absorber (8) and used for purifying ammonia gas separated from the vapor-liquid separator (7).

2. The equipment system for effectively converting and reducing the nitrogen content in dibutyl phthalate wastewater according to claim 1, wherein a circulating pump (4) is arranged between the bottom end and the top end of the hydrolysis kettle (3), a liquid outlet pipe (3.1) is arranged at the bottom end of the hydrolysis kettle (3), the liquid outlet pipe (3.1) is connected with the circulating pump (4) and the rectifying tower (5) in a branching manner, and a circulating pump liquid inlet valve (4.1) is arranged between the circulating pump (4) and the liquid outlet pipe (3.1).

3. The equipment system for effectively converting and reducing the nitrogen content of the dibutyl phthalate wastewater according to claim 1 or 2, wherein a rectification tower air inlet valve (5.1) is arranged in a region where the lower end of the rectification tower (5) is communicated with the liquid outlet pipe (3.1) of the hydrolysis kettle (3).

4. The equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater according to claim 1 or 2, characterized in that an internal heater (11) is arranged in the hydrolysis kettle (3), and a heat medium inlet (12) and a heat medium outlet (13) are respectively arranged on two sides of the internal heater (11).

5. The equipment system for effectively converting and reducing the nitrogen content in dibutyl phthalate wastewater according to claim 3, wherein a feed valve (9) is arranged at the upper end of the hydrolysis kettle (3), a stirrer (10) is arranged in the hydrolysis kettle (3), and a pressure monitor and a temperature monitor are further arranged on the hydrolysis kettle (3).

6. The equipment system for effectively converting and reducing the nitrogen content of the dibutyl phthalate wastewater according to claim 1, wherein the condenser (6) is provided with a cooling liquid inlet (6.1) and a cooling liquid outlet (6.2), and a temperature monitor is arranged between the cooling liquid inlet (6.1) and a pipeline connecting the condenser (6) and the vapor-liquid separator (7).

7. The equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater according to claim 1, wherein the high-efficiency adsorbent is composite gel-filled mesoporous silica, and is prepared by the following steps:

(1) preparing mesoporous silica: placing 0.05-0.1% by mass of hexadecyl trimethyl ammonium bromide solution into a container, adding 28-30wt% by mass of concentrated ammonia water into the solution, continuously stirring for 20-30min, then dripping a mixture of n-hexane and tetraethyl orthosilicate at the speed of 1.0-1.2mL/min, after dripping, continuously stirring for reacting for 10-12h, and after the reaction system gradually turns white; centrifuging, washing with absolute ethyl alcohol, and drying to obtain white hexadecyl trimethyl ammonium bromide-silicon dioxide composite microspheres; ultrasonically dispersing the composite microspheres in a mixed solution of 60-80% by mass of concentrated hydrochloric acid and absolute ethyl alcohol, refluxing for 4-5 hours under magnetic stirring, extracting with acetone to remove hexadecyl trimethyl ammonium bromide, washing with ethyl alcohol, filtering, and drying the obtained white sample in a vacuum oven at 60-80 ℃ for 10-12 hours to finally obtain mesoporous silica microspheres;

(2) activating mesoporous silica: dispersing the silicon dioxide microspheres into dimethylformamide, adding hexamethylene diisocyanate, stirring and reacting for 4-6h at 60-80 ℃, adding 3-triethoxysilyl-1-propylamine, continuously stirring and reacting for 2-4h at 60-70 ℃, centrifuging, and alternately cleaning with absolute ethyl alcohol and ultrapure water to obtain activated mesoporous silicon dioxide;

(3) preparing a filling gel liquid: mixing the composite carbon sol and titanium dioxide according to the mass ratio of 40-60: 1-3, uniformly mixing to obtain composite sol, aging the composite sol for 20-36h, then carrying out solvent replacement on the composite sol for 12-16h by using excessive absolute ethyl alcohol, and then removing the absolute ethyl alcohol to obtain composite gel;

(4) filling mesoporous silica with composite gel: and (3) adding the activated mesoporous silica microspheres obtained in the step (2) into the filling gel liquid obtained in the step (3), stirring for 4-5 hours to enable the gel liquid to be filled into the filling mesoporous silica microspheres, separating the gel liquid from the mesoporous silica microspheres again, drying the filling mesoporous silica microspheres at 60-80 ℃ for 20-30min, carbonizing at 300-600 ℃ to obtain carbonized composite gel filling mesoporous silica, and cleaning and drying the carbonized composite gel filling mesoporous silica to obtain a finished product.

8. The equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater according to claim 7, wherein the volume ratio of the cetyl trimethyl ammonium bromide solution, the concentrated ammonia water, the mixed solution of n-hexane and tetraethyl orthosilicate, and the mixed solution of concentrated hydrochloric acid and anhydrous ethanol in step (1) is 140-160: 3-5: 24-28: 100-; wherein the volume ratio of the normal hexane to the tetraethyl orthosilicate in the mixed solution of the normal hexane and the tetraethyl orthosilicate is 4-5: 1-1.5; the volume ratio of the concentrated hydrochloric acid to the absolute ethyl alcohol in the mixed solution of the concentrated hydrochloric acid and the absolute ethyl alcohol is 1: 98-102; in the step (2), the mass ratio of the silicon dioxide microspheres to the hexamethylene diisocyanate to the 3-triethoxysilyl-1-propylamine is 10: 0.2-0.4: 0.8-1.2.

9. The equipment system for effectively converting and reducing the nitrogen content in the dibutyl phthalate wastewater according to claim 7, wherein the preparation method of the composite carbon sol in the step (3) comprises the following steps: 2-furfural, water-soluble phenolic resin, carbon nano tubes, methyl cellulose, brucite fibers, sodium bicarbonate and water are mixed according to the mass ratio of 5-7: 1: 0.5-0.7: 0.3-0.5: 0.05-0.08: 0.01-0.03: 100, uniformly stirring to obtain a mixed solution, and dropwise adding ammonia water with the concentration of 0.25-0.75mol/L into the mixed solution at the speed of 10-20mL/min under the stirring condition to ensure that the pH value of the mixed solution is more than 8; then reacting for 8-14h at 65-75 ℃ to obtain the composite carbon sol.

10. The equipment system for effectively converting and reducing the nitrogen content in dibutyl phthalate wastewater according to claim 7, wherein the carbonization process of the filled mesoporous silica microspheres in the step (4) is as follows: heating the filled mesoporous silica microspheres to 300-500 ℃ at the speed of 8-12 ℃/min, and keeping the temperature for 30-50 min; then the temperature is raised to 500-600 ℃ at the rate of 18-22 ℃ for carbonization for 50-60 min.

Technical Field

The invention relates to the technical field of plasticizer preparation, in particular to an equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater.

Background

As is well known, plasticizers are added to polymers such as rubber, plastics, paints, etc. during processing to increase their plasticity and flowability and to impart flexibility to the finished products, and are essential additives for the plastics industry. The annual capacity of China reaches 2800kt, the China becomes the first major producing and consuming nation around the world, and the growth momentum is continuously presented. The proportion of phthalic acid esters is again more than 80%. The phthalic anhydride used as raw material for producing phthalic ester is divided into ortho-phthalic anhydride and naphthalene phthalic anhydride, wherein the naphthalene phthalic anhydride accounts for more than 40%. The raw material, process and product analysis of the naphthalene method phthalic anhydride show that the phthalic anhydride contains at least 0.1 percent of phthalimide. Phthalimide is discharged into waste water in the production process of dibutyl phthalate because the phthalimide cannot be converted into a corresponding dibutyl phthalate product. Dibutyl phthalate wastewater cannot treat phthalimide in the traditional plasticizer wastewater treatment process, so that the total nitrogen in the wastewater is high, serious water pollution is caused, and an ecological system is damaged.

The invention discloses a patent number CN201520955765.0 with a patent name of a dibutyl phthalate plasticizer crude ester production system, relates to a plasticizer production device, and particularly relates to a dibutyl phthalate plasticizer crude ester production system. The system comprises an esterification reaction kettle, an esterification tower, a first condenser, an alcohol-water separation tank, an extraction tank and an alcohol storage tank which are sequentially connected, wherein the alcohol storage tank is also connected with the top of the esterification tower; the esterification reaction kettle is also sequentially connected with a second condenser, a buffer tank, a second booster pump, a first mixer, a first ester water separation tank, a second mixer, a second ester water separation tank, a third mixer, a third ester water separation tank and a crude ester tank; the first ester water separation tank is connected with the first alkali water tank; the second ester water separation tank is connected with the second alkali water tank; the third ester water separation tank is connected with the third alkaline water tank; the recycling water tank is respectively connected with the first mixer, the second mixer and the third mixer, and an alkali feeder is arranged on an outlet pipeline of the recycling water tank. The invention has low energy consumption, low labor intensity, high reaction speed and high product purity.

The method has the disadvantages that the total nitrogen content in the wastewater discharged most frequently is too high, and environmental pollution is caused.

Disclosure of Invention

The invention aims to overcome the problem of high total nitrogen content of wastewater in wastewater discharged by plasticizer dibutyl phthalate preparation in the prior art, and provides an equipment system for effectively converting and reducing the nitrogen content of dibutyl phthalate wastewater.

In order to achieve the purpose, the invention adopts the following technical scheme:

the equipment system for effectively converting and reducing the nitrogen content of the dibutyl phthalate wastewater comprises a wastewater tank, a hydrolysis kettle, a rectifying tower, a condenser and a vapor-liquid separator, wherein a wastewater pump is arranged between the bottom end of the wastewater tank and the top end of the hydrolysis kettle, the lower end of the rectifying tower is respectively communicated with the top end of the hydrolysis kettle and the lower end of the hydrolysis kettle, the upper end of the rectifying tower is sequentially connected with the condenser and the vapor-liquid separator to form a closed loop, the vapor-liquid separator is also provided with an ammonia absorber, and the ammonia absorber is filled with a high-efficiency adsorbent and is used for purifying ammonia gas separated from the vapor-liquid separator.

The preparation process comprises the following steps: adding dibutyl phthalate wastewater taking naphthalene phthalic anhydride as a raw material into a hydrolysis kettle from a wastewater tank through a wastewater pump, starting a stirrer of the hydrolysis kettle, adding inorganic strong base through a charging valve, wherein the addition amount of the inorganic strong base keeps the pH value of the dibutyl phthalate wastewater to be more than 11, and heating and refluxing for more than 3 hours under the condition that the pH value is more than 11 in the whole hydrolysis reaction; starting a circulating pump, and opening a heater in a hydrolysis kettle; in the hydrolysis kettle, dibutyl phthalate wastewater and inorganic strong base are used as raw materials, phthalimide is hydrolyzed into phthalate and ammonia gas under the conditions of long-time heating and circulating reflux, and the ammonia gas is absorbed by water to prepare dilute ammonia water. Heating a reaction product in the hydrolysis kettle to be vaporized, enabling the vaporized gas to enter a rectifying tower, enabling the gas to reversely contact with liquid flowing back from the top of the tower in the rectifying tower to enter a condenser, enabling the gas to enter a gas-liquid separator after condensation, carrying out gas-liquid separation on the gas-liquid separator, enabling the liquid to flow back to the rectifying tower from the gas-liquid separator, enabling ammonia gas to escape from the gas-liquid separator and enter an ammonia absorber to prepare low-concentration ammonia water, enabling the ammonia absorber to absorb the low-concentration ammonia water in time, and being capable of avoiding the situation that the ammonia gas is dissolved in the liquid again in the gas-liquid separator and; the high-efficiency adsorbent is arranged in the ammonia gas absorption gas to remove impurity particles and metal ions in the ammonia gas, so that the ammonia water prepared after the ammonia gas is adsorbed has higher purity and less impurity content.

The method can remove the total nitrogen content in the dibutyl phthalate wastewater by fully utilizing the equipment and the reaction principle, and simultaneously prepare the removed nitrogen into the recyclable ammonia water, thereby having the advantages of environmental protection, energy saving, effective realization of pollution-free discharge and raw material cost saving.

Preferably, the bottom and the top of the hydrolysis kettle are communicated and provided with a circulating pump, the bottom of the hydrolysis kettle is provided with a liquid outlet pipe, the liquid outlet pipe is connected with the circulating pump and the rectifying tower in a branch manner, and a circulating pump liquid inlet valve is arranged between the circulating pump and the liquid outlet pipe.

The circulating pump is used for recycling liquid in the reaction kettle, ensures full reaction in the reaction material and ensures the removal effect of nitrogen content in the waste liquid.

Preferably, the lower end of the rectifying tower is provided with an air inlet valve of the rectifying tower in a region communicated with the liquid outlet pipe of the hydrolysis kettle.

Preferably, an inner heater is arranged in the hydrolysis kettle, and a heat medium inlet and a heat medium outlet are respectively arranged on two sides of the inner heater.

When the hydrolysis kettle starts to heat after being charged, the internal heater is started, the heat medium flows in from the heat medium inlet, and after the internal heater is close to the material to be heated and discharges heat to be heated to heat, the heat medium flows out from the heat medium outlet to form a virtuous cycle heating system which is matched with each other, so that the excellent heating cycle system which can be started and stopped immediately after being opened and closed is effectively realized.

Preferably, the upper end of the hydrolysis kettle is provided with a feed valve, a stirrer is arranged in the hydrolysis kettle, and the hydrolysis kettle is further provided with a pressure monitor and a temperature monitor.

The feeding valve provides convenience for adding chemical reaction materials in the hydrolysis kettle, when the hydrolysis kettle starts to work, the stirring stirrer is started, so that the chemical reaction materials in the hydrolysis kettle can be fully mixed, the reaction is more uniform and full, the dibutyl phthalate in the wastewater is fully decomposed, the nitrogen content in the dibutyl phthalate wastewater is fully released in the form of ammonia gas, and finally the purpose of fully reducing the nitrogen content in the dibutyl phthalate wastewater is achieved; the pressure monitor and the temperature monitor the temperature and the pressure condition in the hydrolysis kettle in real time, and adjust and control the temperature and the pressure condition in time, so that the hydrolysis kettle is always in the optimal reaction condition for the chemical reaction raw materials, the reaction effect is ensured, and the safety of the hydrolysis kettle is also ensured.

Preferably, the condenser is provided with a cooling liquid inlet and a cooling liquid outlet respectively, and a temperature monitor is arranged between the cooling liquid inlet and a pipeline connecting the condenser and the vapor-liquid separator.

The condenser cools and liquefies the steam volatilized from the rectifying tower as soon as possible, so that the liquefaction of the steam is accelerated, the liquefied mixed liquid flows back to the gas-liquid separator quickly for gas-liquid separation, and preparation is made for the next step of ammonia gas discharge and absorption; the cooling liquid inlet and the cooling liquid outlet are fully and timely circulated, so that the condensation effect can be better ensured, the steam is quickly cooled and flows back in time, and the nitrogen removal period is shortened; the temperature monitor can properly adjust the flow of the cooling liquid outlet according to the temperature change on the pipeline between the condenser and the gas-liquid separator, when the temperature in the pipeline is overhigh, the flow of the cooling liquid outlet is increased, otherwise, the flow of the cooling liquid outlet is reduced, and the condensation effect of the ammonia water mixed liquid is ensured; the temperature of the top condenser is controlled between 60-70 ℃.

Preferably, the efficient adsorbent is composite gel-filled mesoporous silica, and the preparation steps are as follows:

(1) preparing mesoporous silica: placing 0.05-0.1% by mass of hexadecyl trimethyl ammonium bromide solution into a container, adding 28-30wt% by mass of concentrated ammonia water into the solution, continuously stirring for 20-30min, then dripping a mixture of n-hexane and tetraethyl orthosilicate at the speed of 1.0-1.2mL/min, after dripping, continuously stirring for reacting for 10-12h, and after the reaction system gradually turns white; centrifuging, washing with absolute ethyl alcohol, and drying to obtain white hexadecyl trimethyl ammonium bromide-silicon dioxide composite microspheres; ultrasonically dispersing the composite microspheres in a mixed solution of 60-80% by mass of concentrated hydrochloric acid and absolute ethyl alcohol, refluxing for 4-5 hours under magnetic stirring, extracting with acetone to remove hexadecyl trimethyl ammonium bromide, washing with ethyl alcohol, filtering, and drying the obtained white sample in a vacuum oven at 60-80 ℃ for 10-12 hours to finally obtain mesoporous silica microspheres;

(2) activating mesoporous silica: dispersing the silicon dioxide microspheres into dimethylformamide, adding hexamethylene diisocyanate, stirring and reacting for 4-6h at 60-80 ℃, adding 3-triethoxysilyl-1-propylamine, continuously stirring and reacting for 2-4h at 60-70 ℃, centrifuging, and alternately cleaning with absolute ethyl alcohol and ultrapure water to obtain activated mesoporous silicon dioxide;

(3) preparing a filling gel liquid: mixing the composite carbon sol and titanium dioxide according to the mass ratio of 40-60: 1-3, uniformly mixing to obtain composite sol, aging the composite sol for 20-36h, then carrying out solvent replacement on the composite sol for 12-16h by using excessive absolute ethyl alcohol, and then removing the absolute ethyl alcohol to obtain composite gel;

(4) filling 4.5 mesoporous silica in composite gel: and (3) adding the activated mesoporous silica microspheres obtained in the step (2) into the filling gel liquid obtained in the step (3), stirring for 4-5 hours to enable the gel liquid to be filled into the filling mesoporous silica microspheres, separating the gel liquid from the mesoporous silica microspheres again, drying the filling mesoporous silica microspheres at 60-80 ℃ for 20-30min, carbonizing at 300-600 ℃ to obtain carbonized composite gel filling mesoporous silica, and cleaning and drying the carbonized composite gel filling mesoporous silica to obtain a finished product.

The efficient adsorbent is prepared by mesoporous silica microspheres, which have good adsorption performance and large pore adsorption capacity, the prepared mesoporous silica microspheres have hollow inner surfaces and micro mesopores outside the outer surfaces, the adsorption surface area of the mesoporous silica microspheres can be multiplied, the adsorption capacity of the mesoporous silica microspheres is improved, the adsorption capacity of the mesoporous silica microspheres is obviously improved, but due to the mesopores of the shell layers and the hollow structures inside, the efficient adsorbent also provides wide channels for air flow to pass through while the specific surface area is increased, and when the efficient adsorbent is filled in purified gas or liquid in an esterification tower, the efficient adsorbent can easily pass through the inside of the mesoporous silica microspheres, so that the purification is insufficient; therefore, in the invention, the mesoporous silica microspheres are used as a frame structure, the hollow part in the mesoporous silica microspheres is filled with the composite gel, and the aerogel structure formed after the filled composite gel is dried has stronger adsorption capacity, thereby improving the complexity of the path of purified ammonia gas passing through the microspheres, improving the contact time of the ammonia gas and the microsphere material, finally improving the purification effect and shortening the preparation period.

In the step (1), white hexadecyl trimethyl ammonium bromide-silicon dioxide composite microspheres are synthesized, and hexadecyl trimethyl ammonium bromide components in the microspheres are removed to form a hollow mesoporous structure so as to increase the specific surface area; in the step (2), the mesoporous silica microspheres are subjected to activation grafting of an amino structure, so that the surface activity of the mesoporous silica microspheres is increased, the better integrity of the mesoporous silica microspheres in combination with the composite gel added later is promoted, and the service cycle of the efficient adsorbent is prolonged; the composite sol prepared in the step (3) has a good pore-forming effect, the specific surface area and the adsorption and purification effects of the finally prepared aerogel are increased, and the composite sol is prepared to be alkaline, so that the adsorption rate of the adsorbent to ammonia gas can be reduced; and (4) filling the composite gel into the mesoporous silica microspheres, and carrying out carbonization shaping on the composite gel, so as to finally prepare the high-efficiency adsorbent with good integrity, good formability and good adsorption effect, wherein the mesoporous silica microspheres provide good coating and supporting effects for the composite aerogel, so that the aerogel always maintains a good form, collapse of the aerogel due to mutual extrusion is avoided, the aerogel enriches the adsorption capacity of the mesoporous silica microspheres, ammonia gas is enabled to pass through the high-performance adsorption microspheres, the passing path of the ammonia gas is complicated, the impurity adsorption capacity is increased, and the adsorption to the ammonia gas can be reduced, so that the finally obtained adsorbent has a good selective adsorption impurity removal effect.

Preferably, the volume ratio of the cetyl trimethyl ammonium bromide solution, the concentrated ammonia water, the mixed solution of normal hexane and tetraethyl orthosilicate and the mixed solution of concentrated hydrochloric acid and anhydrous ethanol in the step (1) is 140-160: 3-5: 24-28: 100-; wherein the volume ratio of the normal hexane to the tetraethyl orthosilicate in the mixed solution of the normal hexane and the tetraethyl orthosilicate is 4-5: 1-1.5; the volume ratio of the concentrated hydrochloric acid to the absolute ethyl alcohol in the mixed solution of the concentrated hydrochloric acid and the absolute ethyl alcohol is 1: 98-102; in the step (2), the mass ratio of the silicon dioxide microspheres to the hexamethylene diisocyanate to the 3-triethoxysilyl-1-propylamine is 10: 0.2-0.4: 0.8-1.2.

The 3-triethoxysilyl-1-propylamine is adopted to graft the mesoporous silica in the step (2), so that the grafting efficiency is better, more active sites can be provided for the inner surface and the outer surface of the mesoporous silica, and a solid foundation is laid for the subsequent preparation of the composite gel filled mesoporous silica with good integrity and high binding degree.

Preferably, the preparation method of the composite carbon sol in the step (3) comprises the following steps: 2-furfural, water-soluble phenolic resin, carbon nano tubes, methyl cellulose, brucite fibers, sodium bicarbonate and water are mixed according to the mass ratio of 5-7: 1: 0.5-0.7: 0.3-0.5: 0.05-0.08: 0.01-0.03: 100, uniformly stirring to obtain a mixed solution, and dropwise adding ammonia water with the concentration of 0.25-0.75mol/L into the mixed solution at the speed of 10-20mL/min under the stirring condition to ensure that the pH value of the mixed solution is more than 8; then reacting for 8-14h at 65-75 ℃ to obtain the composite carbon sol.

The carbon nano tube is in a hollow tubular shape and has a pore canal with a nano size, the strength of the material can be improved on the premise that the porosity of the composite carbon sol is not influenced as much as possible, the tenacity of the material can be improved by the brucite fiber, and the sodium bicarbonate has better pore-forming efficiency.

Preferably, the carbonization process of the filled mesoporous silica microspheres in the step (4) is as follows: heating the filled mesoporous silica microspheres to 300-500 ℃ at the speed of 8-12 ℃/min, and keeping the temperature for 30-50 min; then the temperature is raised to 500-600 ℃ at the rate of 18-22 ℃ for carbonization for 50-60 min.

The compound gel that fills adopts progressively heating, and the carbomorphism is accomplished to the form of carbomorphism gradually, and the carbomorphism here is a process step by step, and it is more even to make the inside hole that forms of carbomorphism aerogel, improves the porosity for the carbomorphism is more abundant, promotes its adsorption efficiency, can strengthen the intensity of result again, makes the inside aperture wall of aerogel difficult collapse, and the guarantor type effect is better.

Therefore, the invention has the following beneficial effects:

(1) providing an equipment system for effectively converting and reducing the nitrogen content of the dibutyl phthalate wastewater, hydrolyzing phthalimide by adding inorganic strong base into the dibutyl phthalate wastewater through equipment, reducing total nitrogen, and recovering ammonia gas to realize environment-friendly production of dibutyl phthalate;

(2) the total nitrogen content in the dibutyl phthalate wastewater is removed by fully utilizing related equipment and reaction principles, and the removed nitrogen is prepared into recyclable ammonia water, so that the method is environment-friendly, saves energy, effectively realizes pollution-free discharge and saves raw material cost;

(3) the reaction flow has high nitrogen removal efficiency, simple preparation process, short preparation period and low preparation cost;

(4) the mesoporous silica adsorbent is filled in the composite gel filled in the ammonia absorber to prepare the specific alkaline composite gel, the adsorption of the adsorbent to ammonia gas is reduced while the ammonia gas is purified, impurities in the ammonia gas are removed to improve the purity of the finally prepared ammonia gas, so that the purity of the ammonia water prepared after the ammonia gas is finally adsorbed is higher, the ammonia water can be directly used in fine chemical engineering, and the resource recycling is realized.

Drawings

FIG. 1 is a schematic view of the flow structure of the reaction apparatus of the present invention.

In the figure: 1. a wastewater tank; 2. a waste water pump; 3. a hydrolysis kettle; 3.1, a liquid outlet pipe; 4. a circulation pump; 4.1, a liquid inlet valve of a circulating pump; 5. a rectifying tower; 5.1, an air inlet valve of the rectifying tower; 6. a condenser; 6.1, a cooling liquid inlet; 6.2, a cooling liquid outlet; 7. a vapor-liquid separator; 8. an ammonia absorber; 9. a feed valve; 10. a stirrer; 11. an internal heater; 12. a thermal medium inlet; 13. and a heat medium outlet.

Detailed Description

The invention is further described with reference to specific embodiments.