CN116410087A - Butyl acrylate production wastewater treatment process - Google Patents

Butyl acrylate production wastewater treatment process Download PDF

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Publication number
CN116410087A
CN116410087A CN202310400282.3A CN202310400282A CN116410087A CN 116410087 A CN116410087 A CN 116410087A CN 202310400282 A CN202310400282 A CN 202310400282A CN 116410087 A CN116410087 A CN 116410087A
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butyl acrylate
kettle
esterification
reaction
negative pressure
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潘书铭
邓宇雄
佟刚
赵楚榜
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TAIXING JINJIANG CHEMICAL INDUSTRY CO LTD
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TAIXING JINJIANG CHEMICAL INDUSTRY CO LTD
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Abstract

The invention relates to a butyl acrylate production wastewater treatment process, which is characterized in that the diluted reaction kettle bottom solution is sent into an incinerator for incineration, and most of heat required by production is supplied to the incinerator, and the heat accounts for about 80% of the heat produced, so that zero emission of production wastewater is realized; the vacuum degree is controlled so as to control the boiling point of the liquid, reduce the loss of butyl acrylate and improve the yield and purity of butyl acrylate; the composite carrier is formed by silicon carbide and polyethersulfone, and heteropolyacid, zirconium dioxide and aluminum oxide are loaded, so that the catalyst A has higher anti-fouling, creep resistance and stability while the catalytic activity is improved; through the ultrasonic wave and microwave combination mode, more catalytic active components enter the pore canal, and the load rate is greatly improved. A butyl acrylate production wastewater treatment process comprises the following steps: 1) Depolymerizing the waste heavy component; 2) Esterification reaction; the residue of the esterification kettle waits for rectification and purification; 3) Washing and neutralizing; 4) And (5) rectifying and purifying. Belongs to the technical field of wastewater treatment.

Description

Butyl acrylate production wastewater treatment process
Technical Field
The invention belongs to the technical field of wastewater treatment, and relates to a treatment process of butyl acrylate production wastewater.
Background
The current industrial process for producing butyl acrylate is an acid alcohol esterification method, namely, n-butyl alcohol and acrylic acid are catalyzed by an acid catalyst to produce butyl acrylate, and the industry generally needs to add a catalyst to catalyze the reaction. The production wastewater of butyl acrylate mainly comprises two sources, namely wastewater generated when butyl acrylate is generated by esterification reaction of n-butyl alcohol and acrylic acid, wastewater generated when acid catalyst, acrylic acid and polymerization inhibitor remained in crude ester are neutralized and washed in a neutralizing tower, and waste heavy component generated after butyl acrylate is distilled and purified. The waste water is discharged without treatment, which causes environmental pollution and resource waste.
Whereas the recovery of the discarded heavy fraction, i.e. the industrial butyl acrylate waste oil, generally comprises the steps of depolymerization, esterification, neutralization, light and heavy removal. Firstly, the depolymerization step mainly depolymerizes acrylic acid dimer into corresponding monomers, and the depolymerization step has a great influence on the recovery rate of n-butyl acrylate, so that in order to improve the recovery rate of the effective components of industrial butyl acrylate, shorten the production time, reduce the wastewater discharge, reduce the demands of personnel configuration and the like, the depolymerization step needs to be optimized. The use of the catalyst directly affects the depolymerization efficiency and the recovery rate, and homogeneous catalysts such as toluene sulfonic acid and the like are generally adopted in the industrial depolymerization process, and acrylic acid dimer is catalyzed to crack at high temperature to generate butyl acrylate and butanol. The cracking rate and recovery rate of homogeneous catalytic cracking are lower, when in use, the traditional catalyst is easy to be polluted, the catalytic activity is influenced, and the catalyst is easy to run off due to poor stability, so that the problem of high cost is caused, and the homogeneous catalyst can be stored and sold along with heavy components entering a heavy component storage tank after the cracking reaction or is burnt. And in the heavy component incineration treatment, the sulfur content of the catalyst exceeds the standard of tail gas sulfur and the like.
And secondly, butyl acrylate residual liquid which is insufficiently reacted in the depolymerization step is directly discarded, so that certain materials are wasted.
Disclosure of Invention
The invention aims to provide a treatment process of butyl acrylate production wastewater, which is characterized in that the diluted reaction kettle bottom liquid is sent into an incinerator for incineration, and most of heat required by production is supplied to the incinerator, and the heat accounts for about 80% of the heat produced, so that zero emission of production wastewater is realized; the vacuum degree is controlled so as to control the boiling point of the liquid, reduce the loss of butyl acrylate and improve the yield and purity of butyl acrylate; the composite carrier is formed by silicon carbide and polyethersulfone, and heteropolyacid, zirconium dioxide and aluminum oxide are loaded, so that the catalyst A has higher anti-fouling, creep resistance and stability while the catalytic activity is improved; through the ultrasonic wave and microwave combination mode, more catalytic active components enter the pore canal, and the load rate is greatly improved.
The aim of the invention can be achieved by the following technical scheme:
a butyl acrylate production wastewater treatment process comprises the following steps:
1) Adding the waste heavy components into a reaction kettle, adding a catalyst A, heating, reacting, condensing a gas phase to obtain a reflux stock solution and a reaction kettle bottom solution; acrylic acid and butyl acrylate which are depolymerized by the reaction are in a gas phase and are used for esterification reaction, and noncondensable gas (comprising waste gas generated by feeding) is introduced into a tail gas recovery treatment device for treatment;
2) Adding n-butanol and a reflux stock solution into an esterification kettle, adding a catalyst B and a polymerization inhibitor for reaction, and performing gas phase condensation to obtain an esterification kettle for reflux, wherein the gas phase is water, n-butanol and butyl acrylate, the gas phase is changed into the gas phase in sequence and distilled out from the top, the n-butanol gas phase is subjected to condensation reflux, and the rest gas phase is subjected to condensation and standing to obtain esterification kettle residues (substances such as a small amount of n-butanol, butyl acrylate and butyl acrylate heavy components) and esterification water; the residue of the esterification kettle waits for rectification and purification; washing with water to recover the catalyst B;
3) Transferring the residual materials of the esterification kettle to a neutralization kettle, controlling the temperature, adding sodium hydroxide solution to perform neutralization, washing and stirring, standing, and separating oil from water to obtain coarse materials and neutralization wastewater;
4) And (3) pumping the coarse material to a rectifying kettle through negative pressure, heating, adding a polymerization inhibitor to carry out rectification, wherein the vacuum degree of the first section of negative pressure is-400 to-500 hPa, the vacuum degree of the second section of negative pressure is-780 to-820 hPa, the vacuum degree of the third section of negative pressure is-900 to-1000 hPa, and condensing and refluxing to obtain butyl acrylate and de-weight residual liquid.
As a preferred technical solution of the present invention, in step 1), the discarded heavy component includes 3 parts by weight: 7 acrylic acid heavy component and butyl acrylate heavy component; the heating temperature is 90-110 ℃; the reaction condition is that the reaction is carried out for 10 to 15 hours under normal pressure; in the step 1), the bottom liquid of the reaction kettle is viscous, and is diluted by water and then burnt, and after a certain storage amount is reached, the bottom liquid of the reaction kettle is uniformly sent to an incinerator for burning, and waste heat generated by burning is used for producing most of needed heat, such as procedures of heating, and the like, so that the comprehensive utilization of dangerous waste is achieved, the environment is protected, and the economic benefit is improved; wherein the dilution water is the neutralization wastewater of the step 3).
As a preferable technical scheme of the invention, in the step 2), the mass ratio of the n-butanol to the reflux stock solution is 3-4:10; the catalyst B is p-toluenesulfonic acid, and the polymerization inhibitor is one or two of phenothiazine and copper iodide; the reaction conditions are that the reaction temperature is 80-90 ℃, the negative pressure is minus 850 to minus 350hPa, and the reaction time is 7-10 hours; the standing time is 1-3 h.
As a preferable technical scheme of the invention, in the step 3), the temperature control temperature is 30 ℃, the concentration of sodium hydroxide solution is 8-10%, and the standing time is 1-2 h.
As a preferred embodiment of the invention, in step 3), the sodium hydroxide solution is prepared from sodium hydroxide and the esterification water in step 2).
In the step 4), the rectified material with the first section of negative pressure vacuum degree is material water, and the material water is used for diluting the bottom solution of the reaction kettle in the step 1) or preparing the sodium hydroxide solution in the step 2); the rectifying material with the second section of negative pressure vacuum degree is material n-butyl alcohol, and the material n-butyl alcohol is added into the esterification kettle in the step 2) for esterification reaction; the rectifying material of the third section of negative pressure vacuum degree is butyl acrylate material; the residual liquid after heavy removal is returned to the reaction kettle in the step 1) and is mixed with the waste heavy component for depolymerization.
Further, the scheme of the invention discloses a preparation method of the catalyst A in the step 1), which comprises the following steps:
(1) Mixing heteropoly acid, a porous carrier, zirconium dioxide and aluminum oxide, adding equal volume of deionized water for soaking, carrying out ultrasonic treatment, wherein the ultrasonic frequency is 30-90 Hz, and the treatment time is 10-70 min, so as to obtain a mixed solution;
(2) And (3) placing the mixed solution in a microwave oven for drying treatment for 10-40 min to obtain the catalyst A.
As a preferable technical scheme of the invention, in the step (1), the mass ratio of the heteropolyacid to the porous carrier to the zirconia to the alumina is 15-17: 10 to 15: 20-25: 5 to 7; the heteropolyacid is one or more of phosphotungstic acid, phosphomolybdic acid, silicotungstic acid and silicomolybdic acid.
Further, the scheme of the invention discloses a preparation method of the porous carrier, which comprises the following steps: vacuum sucking the silicon carbide carrier with vacuum degree of 5-20 kPa and sucking time of 5-20 s, coating a layer of polyether sulfone by dipping method, and roasting at 60-100 ℃ for 2-4 h to obtain the porous carrier. As a preferable technical scheme of the invention, the mass ratio of the silicon carbide to the polyethersulfone in the porous carrier is 1-9: 1.
the invention has the beneficial effects that:
1. in the production process, the step 3) wastewater is mixed into the bottom solution of the middle reaction kettle of the reaction kettle, the diluted bottom solution of the reaction kettle is sent into an incinerator for incineration, and the heat generated in the incineration process is utilized for producing most of heat required by production; in the step 2), the esterified water generated by the esterification reaction is used for preparing sodium hydroxide solution, and in the method, the zero emission of the production sewage is achieved.
2. In the step 4), the loss of butyl acrylate is reduced by controlling the vacuum degree and further controlling the boiling point of liquid, moisture and n-butyl alcohol are rectified firstly, and the butyl acrylate content is finally up to 99% after three-stage vacuum degree rectification.
3. The silicon carbide is a porous carrier material, more pore channels are formed through vacuum suction, a composite carrier is formed through coating a polyether sulfone layer, so that heteropolyacid, zirconium dioxide and aluminum oxide are loaded on the composite carrier, the catalyst A is provided with higher anti-fouling, creep resistance and thermal stability through the introduction of the polyether sulfone, and has adsorptivity to metal, the heteropolyacid, zirconium dioxide and aluminum oxide are compounded to provide obvious catalytic activity, the reaction time is greatly shortened, the aluminum oxide is introduced, the activity of the catalyst A is improved, the stability of the catalyst A is enhanced through compounding with the polyether sulfone, and more active components enter the pore channels through ultrasonic combination of microwaves in the preparation process, so that the loading rate is greatly improved.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
In the scheme of the invention, the waste heavy component comprises the following components in parts by weight: 7 acrylic acid heavy component and butyl acrylate heavy component.
In the scheme of the invention, the dosage of the catalyst A is 3% of the mass of the waste heavy component, and the dosage of the polymerization inhibitor is 0.08% of the mass of the waste heavy component.
Waste heavy component
Example 1
The preparation method of the porous carrier comprises the following steps: vacuum sucking the silicon carbide carrier, wherein the vacuum degree is 18kPa, the sucking time is 20s, a layer of polyethersulfone is coated by a dipping method, and the porous carrier is prepared after 4h roasting at 100 ℃, wherein the mass ratio of the silicon carbide to the polyethersulfone in the porous carrier is 5:1.
the preparation method of the catalyst A comprises the following steps:
(1) Mixing phosphotungstic acid, a porous carrier, zirconium dioxide and aluminum oxide, adding equal volume of deionized water for soaking, performing ultrasonic treatment, wherein the ultrasonic frequency is 30Hz, and the treatment time is 10min to obtain a mixed solution; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the zirconium dioxide to the aluminum oxide is 3:2:4:1, a step of;
(2) And (3) placing the mixed solution in a microwave oven for drying treatment for 10min to obtain the catalyst A.
Example 2
The preparation method of the porous carrier comprises the following steps: vacuum sucking the silicon carbide carrier, wherein the vacuum degree is 18kPa, the sucking time is 20s, a layer of polyethersulfone is coated by a dipping method, and the porous carrier is prepared after 4h roasting at 100 ℃, wherein the mass ratio of the silicon carbide to the polyethersulfone in the porous carrier is 5:1.
the preparation method of the catalyst A comprises the following steps:
(1) Mixing phosphotungstic acid, a porous carrier, zirconium dioxide and aluminum oxide, adding equal volume of deionized water for soaking, performing ultrasonic treatment, wherein the ultrasonic frequency is 60Hz, and the treatment time is 40min to obtain a mixed solution; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the zirconium dioxide to the aluminum oxide is 16:13:22:6, preparing a base material;
(2) And (3) placing the mixed solution in a microwave oven for drying treatment for 25min to obtain the catalyst A.
Example 3
The preparation method of the porous carrier comprises the following steps: vacuum sucking the silicon carbide carrier, wherein the vacuum degree is 18kPa, the sucking time is 20s, a layer of polyethersulfone is coated by a dipping method, and the porous carrier is prepared after 4h roasting at 100 ℃, wherein the mass ratio of the silicon carbide to the polyethersulfone in the porous carrier is 5:1.
the preparation method of the catalyst A comprises the following steps:
(1) Mixing phosphotungstic acid, a porous carrier, zirconium dioxide and aluminum oxide, adding equal volume of deionized water for soaking, performing ultrasonic treatment, wherein the ultrasonic frequency is 90Hz, and the treatment time is 70min to obtain a mixed solution; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the zirconium dioxide to the aluminum oxide is 17:15:25:7, preparing a base material;
(2) And (3) placing the mixed solution in a microwave oven for drying treatment for 40min to obtain the catalyst A.
Comparative example 1
The difference from example 2 is that the preparation method of the porous carrier comprises the following steps: vacuum sucking the silicon carbide carrier with vacuum degree of 18kPa and sucking time of 20s, and roasting at 100 deg.c for 4 hr to obtain porous carrier with homogeneous components, preparation steps and parameters.
Comparative example 2
Compared with the embodiment 2, the method is characterized in that in the step (1), after the phosphotungstic acid, the porous carrier and the alumina are mixed, the equal volume of deionized water is added for soaking, the ultrasonic wave frequency is 60Hz, and the treatment time is 40min, so as to obtain a mixed solution; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the alumina is 16:13:6, preparing a base material; the other components, the preparation steps and the parameters are consistent.
Comparative example 3
Compared with the embodiment 2, the method is characterized in that in the step (1), after the phosphotungstic acid, the porous carrier and the zirconium dioxide are mixed, the equal volume of deionized water is added for soaking, the ultrasonic treatment is carried out, the ultrasonic frequency is 60Hz, and the treatment time is 40min, so that a mixed solution is obtained; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the zirconium dioxide is 16:13:22; the other components, the preparation steps and the parameters are consistent.
Comparative example 4
Compared with the embodiment 2, the method is characterized in that in the step (1), after phosphotungstic acid, a porous carrier, zirconium dioxide and aluminum oxide are mixed, equal volume deionized water is added for soaking, ultrasonic treatment is carried out, the ultrasonic frequency is 60Hz, and the treatment time is 40min, so that mixed solution is obtained; wherein the mass ratio of the phosphotungstic acid to the porous carrier to the zirconium dioxide to the aluminum oxide is 16:13:22:6, preparing a base material; (2) And (3) placing the mixed solution in a hot air oven for drying treatment for 25min to obtain the catalyst A. The other components, the preparation steps and the parameters are consistent.
Example 4
A butyl acrylate production wastewater treatment process comprises the following steps:
1) Adding the waste heavy components into a reaction kettle, adding the catalyst A prepared in the example 1, heating to 90 ℃, reacting for 10 hours under normal pressure, and condensing a gas phase to obtain a reflux stock solution and a reaction kettle bottom solution;
2) Adding n-butanol and a reflux stock solution into an esterification kettle according to the mass ratio of 3:10, adding p-toluenesulfonic acid and copper iodide, reacting for 7 hours at the reaction temperature of 80 ℃ and under negative pressure of-850 hPa, taking the gas phase as the reflux of the esterification kettle after condensation, and standing for 1 hour to obtain an esterification kettle residue and esterification water; the dosage of the p-toluenesulfonic acid is 2% of the total mass of the n-butanol and the reflux stock solution;
3) Transferring the residual materials of the esterification kettle to a neutralization kettle, controlling the temperature to be 30 ℃, adding a sodium hydroxide solution with the concentration of 8% for neutralization, washing and stirring, standing for 1h, and separating oil from water to obtain coarse materials and neutralized wastewater;
4) And (3) pumping the coarse material to a rectifying kettle through negative pressure, heating, adding copper iodide, rectifying, wherein the vacuum degree of the first section of negative pressure is-400 hPa, the vacuum degree of the second section of negative pressure is-780 hPa, the vacuum degree of the third section of negative pressure is-900 hPa, and condensing and refluxing to obtain butyl acrylate and heavy-removal residual liquid.
Example 5
A butyl acrylate production wastewater treatment process comprises the following steps:
1) Adding the waste heavy components into a reaction kettle, adding the catalyst A prepared in the example 2, heating to 100 ℃, reacting for 12.5 hours under normal pressure, condensing a gas phase to obtain a reflux stock solution and a reaction kettle bottom solution;
2) Adding n-butanol and a reflux stock solution into an esterification kettle according to the mass ratio of 3.5:10, adding p-toluenesulfonic acid and copper iodide, reacting for 8.5 hours at the reaction temperature of 85 ℃ and under negative pressure of-600 hPa, condensing a gas phase, taking the condensed gas phase as the reflux of the esterification kettle, and standing for 2 hours to obtain an esterification kettle residue and esterification water; the dosage of the p-toluenesulfonic acid is 2% of the total mass of the n-butanol and the reflux stock solution;
3) Transferring the residue of the esterification kettle to a neutralization kettle, controlling the temperature to be 30 ℃, adding a sodium hydroxide solution with the concentration of 9% for neutralization, washing and stirring, standing for 1.5h, and separating oil from water to obtain coarse materials and neutralized wastewater;
4) And (3) pumping the coarse material to a rectifying kettle through negative pressure, heating, adding copper iodide, rectifying, wherein the vacuum degree of the first section of negative pressure is-450 hPa, the vacuum degree of the second section of negative pressure is-800 hPa, the vacuum degree of the third section of negative pressure is-950 hPa, and condensing and refluxing to obtain butyl acrylate and heavy-removal residual liquid.
Example 6
A butyl acrylate production wastewater treatment process comprises the following steps:
1) Adding the waste heavy components into a reaction kettle, adding the catalyst A prepared in the example 3, heating to 110 ℃, reacting for 15 hours under normal pressure, and condensing a gas phase to obtain a reflux stock solution and a reaction kettle bottom solution;
2) Adding n-butanol and a reflux stock solution into an esterification kettle according to the mass ratio of 4:10, adding p-toluenesulfonic acid and copper iodide, reacting for 10 hours at the reaction temperature of 90 ℃ under negative pressure of-350 hPa, taking the gas phase as the reflux of the esterification kettle after condensation, and standing for 3 hours to obtain an esterification kettle residue and esterification water; the dosage of the p-toluenesulfonic acid is 2% of the total mass of the n-butanol and the reflux stock solution;
3) Transferring the residual materials of the esterification kettle to a neutralization kettle, controlling the temperature to be 30 ℃, adding 10% sodium hydroxide solution for neutralization, washing and stirring, standing for 2 hours, and separating oil from water to obtain coarse materials and neutralized wastewater;
4) And (3) pumping the coarse material to a rectifying kettle through negative pressure, heating, adding copper iodide, rectifying, wherein the vacuum degree of the first section of negative pressure is-500 hPa, the vacuum degree of the second section of negative pressure is-820 hPa, the vacuum degree of the third section of negative pressure is-1000 hPa, and condensing and refluxing to obtain butyl acrylate and heavy-removal residual liquid.
Comparative examples 5 to 8
Comparative examples 5 to 8 differ from example 5 in that the catalyst A prepared in example 2 was replaced with the catalyst A prepared in comparative examples 1 to 4, respectively, with the remaining operating steps and parameters unchanged.
The butyl acrylate prepared in examples 4 to 6 and comparative examples 5 to 8 was subjected to yield statistics, and the test results thereof are shown in Table 1.
TABLE 1
Butyl acrylate yield/%
Example 4 99.2
Example 5 99.6
Example 6 99.4
Comparative example 5 66.8
Comparative example 6 70.5
Comparative example 7 63.2
Comparative example 8 84
As can be seen from the test results in Table 1, in examples 4 to 6, compared with comparative examples 5 to 8, the catalyst A has higher anti-fouling, creep resistance and stability by forming a composite carrier by silicon carbide and polyethersulfone and loading heteropolyacid, zirconium dioxide and aluminum oxide; through the ultrasonic wave and microwave combination mode, more catalytic active components enter the pore canal, so that the loading rate is greatly improved, and the catalytic activity of the catalyst A is remarkably improved.
In addition, the solution of the invention is that the diluted bottom solution of the reaction kettle is sent into the incinerator for incineration, the heat of the bottom solution is used for producing most of the heat required by production, and the heat accounts for about 80 percent of the heat produced by the esterification reaction, and the esterified water produced by the esterification reaction is used for preparing sodium hydroxide solution, thus realizing zero emission of production sewage; the vacuum degree is controlled to further control the boiling point of the liquid, so that the loss of butyl acrylate is reduced, and the yield and purity of butyl acrylate are improved.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.

Claims (10)

1. The butyl acrylate production wastewater treatment process is characterized by comprising the following steps of:
1) Adding the waste heavy components into a reaction kettle, adding a catalyst A, heating, reacting, condensing a gas phase to obtain a reflux stock solution and a reaction kettle bottom solution;
2) Adding n-butanol and a reflux stock solution into an esterification kettle, adding a catalyst B and a polymerization inhibitor, reacting, condensing a gas phase, refluxing the gas phase as the esterification kettle, and standing to obtain an esterification kettle residue and esterification water;
3) Transferring the residual materials of the esterification kettle to a neutralization kettle, controlling the temperature, adding sodium hydroxide solution to perform neutralization, washing and stirring, standing, and separating oil from water to obtain coarse materials and neutralization wastewater;
4) And (3) pumping the coarse material to a rectifying kettle through negative pressure, heating, adding a polymerization inhibitor to carry out rectification, wherein the vacuum degree of the first section of negative pressure is-400 to-500 hPa, the vacuum degree of the second section of negative pressure is-780 to-820 hPa, the vacuum degree of the third section of negative pressure is-900 to-1000 hPa, and condensing and refluxing to obtain butyl acrylate and de-weight residual liquid.
2. The process for treating butyl acrylate production wastewater according to claim 1, which is characterized in that: in the step 1), the waste heavy component comprises the following components in parts by weight: 7 acrylic acid heavy component and butyl acrylate heavy component; the heating temperature is 90-110 ℃; the reaction condition is that the reaction is carried out for 10 to 15 hours under normal pressure; in the step 1), the bottom solution of the reaction kettle is diluted by water and then burnt, wherein the dilution water is the neutralization wastewater in the step 3).
3. The process for treating butyl acrylate production wastewater according to claim 1, which is characterized in that: in the step 2), the mass ratio of the n-butanol to the reflux stock solution is 3-4:10; the catalyst B is p-toluenesulfonic acid, and the polymerization inhibitor is one or two of phenothiazine and copper iodide; the reaction conditions are that the reaction temperature is 80-90 ℃, the negative pressure is minus 850 to minus 350hPa, and the reaction time is 7-10 hours; the standing time is 1-3 h.
4. The process for treating butyl acrylate production wastewater according to claim 1, which is characterized in that: in the step 3), the temperature is controlled to be 30 ℃, the concentration of sodium hydroxide solution is 8-10%, and the standing time is 1-2 h.
5. The process for treating butyl acrylate production wastewater according to claim 1, which is characterized in that: in step 3), sodium hydroxide solution is prepared from sodium hydroxide and the esterification water in step 2).
6. The process for treating butyl acrylate production wastewater according to claim 1, which is characterized in that: in the step 4), the rectifying material with the first section of negative pressure vacuum degree is material water, and the material water is used for diluting the bottom solution of the reaction kettle in the step 1) or preparing the sodium hydroxide solution in the step 2); the rectifying material with the second section of negative pressure vacuum degree is material n-butyl alcohol, and the material n-butyl alcohol is added into the esterification kettle in the step 2) for esterification reaction; the rectifying material of the third section of negative pressure vacuum degree is butyl acrylate material; the residual liquid after heavy removal is returned to the reaction kettle in the step 1) and is mixed with the waste heavy component for depolymerization.
7. The process for treating wastewater from butyl acrylate production according to claim 1, wherein the preparation method of the catalyst A comprises the following steps:
(1) Mixing heteropoly acid, a porous carrier, zirconium dioxide and aluminum oxide, adding equal volume of deionized water for soaking, carrying out ultrasonic treatment, wherein the ultrasonic frequency is 30-90 Hz, and the treatment time is 10-70 min, so as to obtain a mixed solution;
(2) And (3) placing the mixed solution in a microwave oven for drying treatment for 10-40 min to obtain the catalyst A.
8. The process for treating butyl acrylate production wastewater according to claim 7, wherein the process comprises the following steps: in the step (1), the mass ratio of the heteropolyacid to the porous carrier to the zirconia to the alumina is 15-17: 10 to 15: 20-25: 5 to 7; the heteropolyacid is one or more of phosphotungstic acid, phosphomolybdic acid, silicotungstic acid and silicomolybdic acid.
9. The process for treating wastewater from butyl acrylate production according to claim 7, wherein the preparation method of the porous carrier comprises the following steps: vacuum sucking the silicon carbide carrier with vacuum degree of 5-20 kPa and sucking time of 5-20 s, coating a layer of polyether sulfone by dipping method, and roasting at 60-100 ℃ for 2-4 h to obtain the porous carrier.
10. The process for treating butyl acrylate production wastewater according to claim 9, wherein the process comprises the following steps: the mass ratio of the silicon carbide to the polyethersulfone in the porous carrier is 1-9: 1.
CN202310400282.3A 2023-04-14 2023-04-14 Butyl acrylate production wastewater treatment process Pending CN116410087A (en)

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王新军: "利用丙烯酸酯重组分生产丙烯酸丁酯工艺研究", 《山东化工》, vol. 49, no. 9, pages 51 - 52 *

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