CN111559816A - Method for treating wastewater of methyl methacrylate device - Google Patents
Method for treating wastewater of methyl methacrylate device Download PDFInfo
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- CN111559816A CN111559816A CN201910112684.7A CN201910112684A CN111559816A CN 111559816 A CN111559816 A CN 111559816A CN 201910112684 A CN201910112684 A CN 201910112684A CN 111559816 A CN111559816 A CN 111559816A
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- wastewater
- methyl methacrylate
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- treating
- plant
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 239000002351 wastewater Substances 0.000 title claims abstract description 112
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000003513 alkali Substances 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- MWFMGBPGAXYFAR-UHFFFAOYSA-N 2-hydroxy-2-methylpropanenitrile Chemical compound CC(C)(O)C#N MWFMGBPGAXYFAR-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000003672 processing method Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000012856 packing Methods 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention provides a method for treating wastewater of a methyl methacrylate device. The processing method comprises the following steps: adjusting the pH value of the wastewater of the methyl methacrylate device to 9.7-10.3 by using alkali; and introducing the methyl methacrylate device wastewater after the pH value is adjusted into a rectifying tower for rectification so as to remove methyl methacrylate in the wastewater. The treatment method provided by the invention can effectively solve the problem that methyl methacrylate contained in the wastewater is easy to polymerize in the heating process, and the treated wastewater meets the biochemical treatment requirement.
Description
Technical Field
The invention relates to the field of chemical wastewater treatment, in particular to a method for treating wastewater of a methyl methacrylate device.
Background
Methyl methacrylate is produced by an acetone cyanohydrin method (ACH method), and the device comprises a tail gas blower, a refining delayer, a steam jet pump and other equipment which generate waste water in the normal operation process, wherein the waste water has high COD value and strong acidity, and mainly contains organic matters such as methanol, acetone, methyl methacrylate and the like through chemical analysis, the COD value is mainly contributed by the organic matters, and the COD value of the waste water can be reduced only by removing the organic matters in the waste water. Methyl methacrylate contained in the wastewater begins to polymerize when the temperature reaches 60 ℃ under the normal-pressure heating condition, and a common methyl methacrylate polymerization inhibitor cannot achieve a good polymerization inhibition effect in the wastewater heating process due to complex wastewater composition and obvious strong acidity, so that if methyl methacrylate in the wastewater undergoes a polymerization phenomenon, the wastewater is turbid and has polymers, and biochemical treatment cannot be performed.
Taking a methyl methacrylate device of a certain factory in China as an example, a matched biochemical treatment device requires that wastewater can be biochemically treated to meet three conditions:
(1) the wastewater is clear and has no suspended matters;
(2) the COD value is lower than 20000 mg/L;
(3) the pH is neutral or weakly acidic.
The device produces 9 tons of waste water per hour, and waste water COD is up to 238000mg/L, and pH value 2.38 shows strong acidity, can't directly carry out biochemical treatment, mainly uses the natural gas to burn this part of waste water as fuel at present, produces waste gas in the waste water combustion process, and waste water treatment cost is high and not environmental protection.
Disclosure of Invention
The invention mainly aims to provide a method for treating methyl methacrylate device wastewater, which solves the problem that methyl methacrylate contained in the wastewater is easy to polymerize in the heating process, so that the treated wastewater meets the biochemical treatment requirement.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for treating wastewater of a methyl methacrylate plant, comprising the steps of: adjusting the pH value of the wastewater of the methyl methacrylate device to 9.7-10.3 by using alkali; and introducing the methyl methacrylate device wastewater after the pH value is adjusted into a rectifying tower for rectification so as to remove methyl methacrylate in the wastewater.
Further, in the rectification process, the operation pressure is normal pressure, the temperature of a tower kettle is controlled to be 100-102 ℃, the temperature of a tower top is controlled to be 71-73 ℃, and the reflux ratio is controlled to be 3: 1-5: 1.
Further, in the rectification process, the temperature of a tower kettle is controlled to be 101 ℃, the temperature of a tower top is controlled to be 72 ℃, and the reflux ratio is controlled to be 3: 1-5: 1.
Furthermore, the number of theoretical plates of the rectifying tower is 25-27.
Further, the rectifying tower comprises a rectifying section and a stripping section, wherein the number of theoretical plates of the rectifying section is 19-21, and the number of theoretical plates of the stripping section is 5-7.
Further, the number of theoretical plates of the rectifying section was 20, and the number of theoretical plates of the stripping section was 6.
Further, in the process of adjusting the pH value of the wastewater of the methyl methacrylate plant, the pH value was adjusted to 10.
Further, in the process of adjusting the pH value of the wastewater of the methyl methacrylate device, the adopted alkali is sodium hydroxide and/or potassium hydroxide.
Furthermore, the wastewater of the methyl methacrylate device is the wastewater generated in the operation process of the methyl methacrylate device produced by the acetone cyanohydrin method.
By applying the technical scheme of the invention, the pH value of the wastewater of the methyl methacrylate device is adjusted to 9.7-10.3, and then the wastewater is rectified. In the rectification process, one part of methyl methacrylate contained in the wastewater can react with alkali to generate methacrylate, and the other part of methyl methacrylate can be azeotroped with methanol in the wastewater to the tower top for removal. In the process, if the added alkali amount is too much, the COD value of the treated wastewater is unqualified, and if the added alkali amount is less, the wastewater is polymerized in the heating process, but the pH value of the wastewater is adjusted to 9.7-10.3 by adding the alkali, so that the polymerization of methyl methacrylate can be inhibited, and the influence of too much alkali on the COD is avoided. In a word, the treatment method provided by the invention can effectively solve the problem that methyl methacrylate contained in the wastewater is easy to polymerize in the heating process, and the treated wastewater meets the biochemical treatment requirement.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
The "methyl methacrylate plant wastewater" in the invention refers to wastewater with a high COD value generated in a device (including a device tail gas blower, a refining delayer, a steam jet pump and other equipment) for producing methyl methacrylate by an acetone-cyanohydrin method (ACH method) in the normal operation process.
As described in the background section, methyl methacrylate contained in the wastewater of the methyl methacrylate plant is easy to polymerize in the heating process, and the wastewater treated by the existing treatment process cannot meet the requirements of biochemical treatment.
In order to solve the above problems, the present invention provides a method for treating wastewater from a methyl methacrylate plant, comprising the steps of: adjusting the pH value of the wastewater of the methyl methacrylate device to 9.7-10.3 by using alkali; and introducing the methyl methacrylate device wastewater after the pH value is adjusted into a rectifying tower for rectification so as to remove methyl methacrylate in the wastewater.
In the rectification process, one part of methyl methacrylate contained in the wastewater can react with alkali to generate methacrylate, and the other part of methyl methacrylate can be azeotroped with methanol in the wastewater to the tower top for removal. In the process, if the added alkali amount is too much, the COD value of the treated wastewater is unqualified, and if the added alkali amount is less, the wastewater is polymerized in the heating process, but the pH value of the wastewater is adjusted to 9.7-10.3 by adding the alkali, so that the polymerization of methyl methacrylate can be inhibited, and the influence of too much alkali on the COD is avoided. In a word, the treatment method provided by the invention can effectively solve the problem that methyl methacrylate contained in the wastewater is easy to polymerize in the heating process, and the treated wastewater meets the biochemical treatment requirement.
In order to further improve the removal effect of methyl methacrylate in the rectification process, in a preferred embodiment, the operation pressure in the rectification process is normal pressure, the temperature of a tower kettle is controlled to be 100-102 ℃, the temperature of a tower top is controlled to be 71-73 ℃, and the reflux ratio is controlled to be 3: 1-5: 1. More preferably, in the rectification process, the temperature of a tower kettle is controlled to be 101 ℃, the temperature of a tower top is controlled to be 72 ℃, and the reflux ratio is controlled to be 3: 1-5: 1.
In order to further improve the removal effect of methyl methacrylate in the rectification process, in a preferred embodiment, the number of theoretical plates of the rectification column is 25-27. More preferably, the rectifying tower comprises a rectifying section and a stripping section, wherein the number of theoretical plates of the rectifying section is 19-21, and the number of theoretical plates of the stripping section is 5-7. Further preferably, the number of theoretical plates of the rectifying section is 20, and the number of theoretical plates of the stripping section is 6.
In order to further improve the removal effect of methyl methacrylate in the rectification process and simultaneously reduce the COD value of the treated wastewater, in a preferred embodiment, the pH value is adjusted to 10 in the process of adjusting the pH value of the wastewater of the methyl methacrylate device.
In a preferred embodiment, the base used in the adjustment of the pH of the wastewater from the methyl methacrylate plant is sodium hydroxide and/or potassium hydroxide.
In a preferred embodiment, the methyl methacrylate plant waste water is waste water produced during the operation of a plant for the production of methyl methacrylate by the acetone cyanohydrin process.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Taking the waste water of methyl methacrylate device of a certain factory in China, and adjusting the PH value of the waste water of methyl methacrylate to 10 by adding alkali.
The rectification process comprises the steps of continuously sampling 10 times to analyze the COD value and the PH value of the wastewater, wherein the total height of the packing of the rectification tower is 52cm (26 trays), the height of a rectification section is 12cm (6 trays), the height of a stripping section is 40cm (20 trays), the temperature of a tower kettle is 101 ℃, the temperature of a tower top is 72 ℃, the reflux ratio is 4:1, the operation pressure is normal pressure, and the results are shown in Table 1.
TABLE 1 COD, PH and appearance of the wastewater
The data in Table 1 show that the treated wastewater is continuously sampled for 10 times, the average value of COD is 14500, the average value of PH is 6.86, the appearance of the wastewater is clear and transparent, and the requirements of biochemical treatment of the device are met.
Example 2
Taking the waste water of methyl methacrylate device of a certain factory in China, and adjusting the pH value of the waste water of methyl methacrylate to 9.7 by adding alkali.
The rectification process comprises the steps of continuously sampling 10 times to analyze the COD value and the PH value of the wastewater, wherein the total height of the packing of the rectification tower is 52cm (26 trays), the height of a rectification section is 12cm (6 trays), the height of a stripping section is 40cm (20 trays), the temperature of a tower kettle is 101 ℃, the temperature of a tower top is 72 ℃, the reflux ratio is 4:1, the operation pressure is normal pressure, and the results are shown in Table 2.
TABLE 2 COD, PH and appearance of the wastewater
The data in Table 2 show that the treated wastewater is continuously sampled for 10 times, the average COD value is 12920, the average pH value is 6.46, the wastewater has muddy appearance and trace suspended matters, and the biochemical treatment requirements of the device are basically met.
Example 3
The pH of the methyl methacrylate wastewater was adjusted to 10.3 by adding alkali.
The rectification process comprises the steps of continuously sampling 10 times to analyze the COD value and the PH value of the wastewater, wherein the total height of the packing of the rectification tower is 52cm (26 trays), the height of a rectification section is 12cm (6 trays), the height of a stripping section is 40cm (20 trays), the temperature of a tower kettle is 101 ℃, the temperature of a tower top is 72 ℃, the reflux ratio is 4:1, the operation pressure is normal pressure, and the results are shown in Table 3.
TABLE 3 COD, PH and appearance of the wastewater
The data in Table 3 show that the treated wastewater is sampled for 10 times continuously, the average value of COD is 18200, the average value of PH is 6.98, the appearance of the wastewater is clear and transparent, but the average value of COD of the wastewater is close to 20000mg/L, the risk that the COD exceeds 20000mg/L due to process fluctuation exists, and the biochemical treatment requirements of the device are basically met.
Example 4
Taking the waste water of methyl methacrylate device of a certain factory in China, and adjusting the PH value of the waste water of methyl methacrylate to 10 by adding alkali.
The rectification process comprises the steps of continuously sampling 10 times to analyze the COD value and the PH value of the wastewater, wherein the total height of the packing of the rectification tower is 50cm (25 tower plates), the height of a rectification section is 10cm (5 tower plates), the height of a stripping section is 40cm (20 tower plates), the temperature of a tower kettle is 102 ℃, the temperature of a tower top is 71 ℃, the reflux ratio is 5:1, the operation pressure is normal pressure, and the results are shown in Table 4.
TABLE 4 COD, PH and appearance of the wastewater
The data in Table 4 show that the treated wastewater was sampled 10 times continuously, the average COD value was 14500, the average pH value was 6.87, the wastewater appearance was slightly turbid and had a trace of suspended matter, which basically satisfied the biochemical treatment requirements of the apparatus.
Comparative example 1
Taking the waste water of the methyl methacrylate device of a certain factory in China, and adjusting the pH value of the waste water of the methyl methacrylate to 9.5 by adding alkali.
The rectification process comprises the steps of continuously sampling 10 times to analyze the COD value and the PH value of the wastewater, wherein the total height of the packing of the rectification tower is 52cm (26 trays), the height of a rectification section is 12cm (6 trays), the height of a stripping section is 40cm (20 trays), the temperature of a tower kettle is 101 ℃, the temperature of a tower top is 72 ℃, the reflux ratio is 4:1, the operation pressure is normal pressure, and the results are shown in Table 5.
TABLE 5 COD, PH and appearance of the wastewater
The data in Table 5 show that the treated wastewater is continuously sampled for 10 times, the average value of COD is 14308, the average value of PH is 6.44, but the wastewater is turbid in appearance and has a large amount of suspended matters, and the biochemical treatment requirements of the device are basically met.
From the above description, it can be seen that the methyl methacrylate wastewater treatment process provided by the invention has the following advantages:
(1) the wastewater after the alkali is added is heated and does not polymerize in the normal pressure rectification process;
(2) after the process is further optimized, the treated tower kettle wastewater is clear and transparent;
(3) after the process is further optimized, the average COD value of the treated tower kettle wastewater is 14500mg/L, which is lower than the requirement of 20000 mg/L;
(4) after the process is further optimized, the average pH value of the treated tower kettle wastewater is 6.86 and is close to neutral, and biochemical treatment can be carried out without adjusting the pH value.
(5) The treatment process is green and environment-friendly, and no waste gas is generated.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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.
Claims (9)
1. A method for treating wastewater of a methyl methacrylate device is characterized by comprising the following steps:
adjusting the pH value of the methyl methacrylate device wastewater to 9.7-10.3 by adopting alkali;
and introducing the methyl methacrylate device wastewater after the pH value is adjusted into a rectifying tower for rectification so as to remove methyl methacrylate in the wastewater.
2. The method for treating methyl methacrylate device wastewater as claimed in claim 1, wherein in the rectification process, the operation pressure is normal pressure, the temperature of the tower bottom is controlled to be 100-102 ℃, the temperature of the tower top is controlled to be 71-73 ℃, and the reflux ratio is controlled to be 3: 1-5: 1.
3. The method for treating the wastewater of the methyl methacrylate plant as claimed in claim 2, wherein in the rectification process, the temperature of the tower bottom is controlled to be 101 ℃, the temperature of the tower top is controlled to be 72 ℃, and the reflux ratio is controlled to be 3: 1-5: 1.
4. The method of treating methyl methacrylate plant wastewater according to claim 2 or 3, wherein the number of theoretical plates of the rectifying column is 25 to 27.
5. The method for treating methyl methacrylate plant wastewater according to claim 4, wherein the rectifying column comprises a rectifying section and a stripping section, wherein the number of theoretical plates of the rectifying section is 19 to 21, and the number of theoretical plates of the stripping section is 5 to 7.
6. The method according to claim 5, wherein the number of theoretical plates in the rectifying section is 20, and the number of theoretical plates in the stripping section is 6.
7. The method for treating methyl methacrylate plant wastewater according to any one of claims 1 to 3, wherein in the step of adjusting the pH of the methyl methacrylate plant wastewater, the pH is adjusted to 10.
8. The method for treating methyl methacrylate plant wastewater according to any one of claims 1 to 3, wherein the alkali used in the process of adjusting the pH of the methyl methacrylate plant wastewater is sodium hydroxide and/or potassium hydroxide.
9. The method for treating wastewater of a methyl methacrylate plant according to any one of claims 1 to 3, wherein the wastewater of the methyl methacrylate plant is wastewater generated during the operation of a plant for producing methyl methacrylate by an acetone cyanohydrin method.
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| CN201910112684.7A CN111559816B (en) | 2019-02-13 | 2019-02-13 | Method for treating wastewater of methyl methacrylate device |
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