CN113443750A - Experimental method for treating esterification reaction wastewater - Google Patents
Experimental method for treating esterification reaction wastewater Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C02F2101/00—Nature of the contaminant
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- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to an esterification reaction wastewater treatment experimental method, which comprises the following steps of firstly, preparing a reaction solution required by an experiment; adding wastewater of an esterification reaction in production of a bio-based plasticizer into a first reaction tank for waiting for treatment; adding FeSO 4.7H 2O and wastewater of epoxidation reaction into the first reaction tank for reaction to obtain a reaction mixed solution, adding the reaction solution for flocculation reaction, and taking supernate for subsequent treatment; adding NaOH solution into the second reaction tank, removing iron ions in the supernatant, stirring uniformly, standing for precipitation, and taking the supernatant for detection of each index; and recording the experimental result. The invention has the advantages that: the wastewater of the esterification reaction and the wastewater of the epoxidation reaction are combined, the COD value of the wastewater of the esterification reaction can be effectively reduced, the concentration of hydrogen peroxide in the wastewater of the epoxidation reaction can be diluted, the simultaneous treatment of the wastewater of two places is realized, and the method is very convenient.
Description
Technical Field
The invention relates to the field of production of bio-based plasticizers, and particularly relates to an experimental method for treatment of esterification reaction wastewater.
Background
At present, the production flow of the existing bio-based plasticizer is generally as follows: esterification is carried out on vegetable oleic acid alcohol to obtain an esterified substance, and the esterified substance is subjected to epoxidation to obtain the required bio-based plasticizer product. In the production process, a large amount of wastewater is generated in the processes of esterification and epoxidation, the wastewater of esterification contains esterified substances, alcohols, vegetable oleic acid and the like, the wastewater of epoxidation contains 20% of hydrogen peroxide, organic acids and the like, and the wastewater after the two reactions cannot be directly discharged.
When handling the waste water to esterification reaction, waste water COD is high, lead to BOD and COD ratio very little, and the biodegradability is not good, difficult biodegradable, can't handle with the activated sludge method, and adopt ferrous and 30% hydrogen peroxide solution to handle, with the COD value in reducing its waste water, when handling, still need add acid treatment to waste water earlier, with the PH value that reduces waste water, however, can make the hydrogen peroxide solution that contains high concentration in the waste water like this, the unable accurate control waste water treatment index.
When the wastewater of the epoxidation reaction is treated, the wastewater contains 20% of hydrogen peroxide, and if the wastewater is directly sent to a sewage treatment station for treatment, a biochemical system of the sewage treatment station is easy to be paralyzed, so that the wastewater needs to be diluted to below 5% by tap water before being sent to the sewage treatment station, and is diluted to 5% from nearly 20%, a large amount of tap water is needed, and the treatment capacity of the wastewater is increased.
Disclosure of Invention
The invention aims to provide an experimental method for treating esterification reaction wastewater, which can effectively reduce COD in the esterification reaction wastewater.
In order to solve the technical problems, the technical scheme of the invention is as follows: an experimental method for treating esterification reaction wastewater has the innovation points that: comprises the following steps
S1: firstly, preparing reaction solution required by an experiment, wherein the reaction solution comprises 10% PAC solution, 2% o PAM solution and 10% NaOH solution;
s2: adding esterification wastewater in production of a bio-based plasticizer into a first reaction tank for waiting for treatment, and waiting epoxidation wastewater for standby application, wherein the esterification wastewater contains an esterified substance, alcohol and vegetable oleic acid, and the epoxidation wastewater contains 20% of hydrogen peroxide and organic acid;
s3: adding FeSO 4.7H 2O into the first reaction tank, dropwise adding epoxidation wastewater into the first reaction tank, uniformly stirring by using a glass rod, standing, and reacting for 2-4 hours to obtain a reaction mixed solution;
s4: dripping 10% NaOH solution into the first reaction tank, adjusting the pH value of the reaction mixed solution to 8-9, dripping 10% PAC solution and 2 thousandth PAM solution into the first reaction tank, performing flocculation reaction on the reaction mixed solution, and taking supernatant in the first reaction tank for subsequent treatment after the reaction is completely precipitated;
s5: after the reaction is finished, taking the supernatant into a second reaction tank, adding NaOH solution into the second reaction tank, adjusting the pH value of the supernatant back to 10 to remove iron ions in the supernatant, uniformly stirring, standing for precipitation, and taking the supernatant for detection of each index;
s6: and recording the experimental result, wherein the type of the added medicine, the dosage, the experimental process, the reaction and precipitation time, the sludge amount and the condition of the supernatant in the experimental process are recorded, and a picture of the experimental process is left.
Further, in the step S3, the addition amount of FeSO 4.7H 2O is 8-30% of the amount of the esterification reaction wastewater.
Further, in the step S3, the addition amount of the wastewater of the epoxidation reaction is 30-60% of the amount of the wastewater of the esterification reaction, and the addition speed of the wastewater of the epoxidation reaction is 150 kg/h-300 kg/h per ton of the wastewater.
Further, in the step S4, the dropping speed of the PAC solution is 0.05 kg/h-0.25 kg/h per ton of wastewater, and the dropping amount of the PAC solution is 0.1% -0.5% of the amount of the esterification reaction wastewater.
Further, in the step S4, the dropping speed of the PAM solution is 0.45 kg/h-1.25 kg/h per ton of wastewater, and the dropping amount of the PAM solution is 1% -3% of the amount of the esterification reaction wastewater.
The invention has the advantages that: in the method, when the wastewater is treated, the wastewater of the esterification reaction and the wastewater of the epoxidation reaction are combined through the matching of all the steps, and the COD value of the wastewater of the esterification reaction can be effectively reduced through the matching of a plurality of reaction solutions, and the concentration of hydrogen peroxide in the wastewater of the epoxidation reaction can be diluted, so that the simultaneous treatment of two kinds of wastewater is realized, the method is very convenient, the B/C ratio of the wastewater is reduced, and the biochemical property of the wastewater is improved.
In the experiment, FeSO4 & 7H2O and hydrogen peroxide solution are firstly used for reacting the wastewater, and then the wastewater is flocculated by the reaction solution, so that the precipitation of substances generated by the reaction can be accelerated, and the COD value of the wastewater can be further reduced.
The wastewater of the esterification reaction and the wastewater of the epoxidation reaction are combined, and the wastewater of the epoxidation reaction contains hydrogen peroxide to treat the esterification wastewater, so that the raw material hydrogen peroxide for treating the esterification wastewater is saved, the PH of the wastewater is not required to be adjusted due to the organic acid contained in the wastewater of the epoxidation reaction, and the problem of additionally treating the wastewater of high-concentration hydrogen peroxide is solved.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the scope of the embodiments described herein.
The esterification reaction wastewater treatment experimental method is realized by the following steps:
s1: firstly, reaction solutions required by experiments are prepared, wherein the reaction solutions comprise 10% PAC solution, 2% PAM solution and 10% NaOH solution.
S2: adding esterification wastewater in the production of the bio-based plasticizer into a first reaction tank for waiting to be treated, and waiting epoxidation wastewater for later use, wherein the esterification wastewater contains an esterified substance, alcohol and vegetable oleic acid, and the epoxidation wastewater contains 20% of hydrogen peroxide and organic acid.
S3: adding FeSO4 & 7H2O into the first reaction tank, dropwise adding epoxidation reaction wastewater into the first reaction tank, uniformly stirring by using a glass rod, standing, and reacting for 2-4 hours to remove organic matters such as alcohol and vegetable oleic acid contained in the esterification reaction wastewater to obtain a reaction mixed solution.
In the steps, the addition amount of FeSO4 & 7H2O is 8% -30% of the amount of the esterification reaction wastewater, the addition amount of the epoxidation reaction wastewater is 30-60% of the amount of the esterification reaction wastewater, and the addition speed of the epoxidation reaction wastewater is 150 kg/H-300 kg/H per ton of wastewater.
S4: and (2) dropwise adding a 10% NaOH solution into the first reaction tank, adjusting the pH value of the reaction mixed solution to 8-9, dropwise adding a 10% PAC solution and a 2% PAM solution into the first reaction tank, so as to perform flocculation reaction on the reaction mixed solution, precipitate ferric hydroxide and some grease generated by the reaction, and taking the supernatant in the first reaction tank for subsequent treatment after the reaction precipitation is complete.
In the steps, the dropping speed of the PAC solution is 0.05 kg/h-0.25 kg/h per ton of wastewater, the dropping amount of the PAC solution is 0.1-0.5% of the amount of the esterification reaction wastewater, the dropping speed of the PAM solution is 0.45 kg/h-1.25 kg/h per ton of wastewater, and the dropping amount of the PAM solution is 1-3% of the amount of the esterification reaction wastewater.
S5: and after the reaction is finished, taking the supernatant into a second reaction tank, adding NaOH solution into the second reaction tank, adjusting the pH value of the supernatant back to 10 to remove iron ions in the supernatant, uniformly stirring, standing for precipitation, and taking the supernatant for detection of each index.
S6: and recording the experimental result, wherein the type of the added medicine, the dosage, the experimental process, the reaction and precipitation time, the sludge amount and the condition of the supernatant in the experimental process are recorded, and a picture of the experimental process is left.
The experimental treatment according to the above procedure is performed by a plurality of different examples, and experimental analysis and comparison of data are performed, wherein in the first to fourth examples, 30% hydrogen peroxide is added for treatment, so that the ph of the wastewater from the esterification reaction is required to be adjusted to 2-4 before the first to fourth examples, and in the fifth to seventh examples, the wastewater from the epoxidation reaction in the present invention is treated, so that the ph of the wastewater from the esterification reaction is not required to be adjusted in advance.
Example one
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 24.53g, the addition amount of 30% hydrogen peroxide solution is 90ML, the reaction is carried out for 2 hours, the obtained reaction mixed solution is sampled and detected, the COD content is 56306mg/L, after flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 54195mg/L, and no BOD is detected.
Example two
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 49.06g, the addition amount of 30% hydrogen peroxide solution is 181ML, the reaction is carried out for 2 hours, the obtained reaction mixed solution is sampled and detected, the COD content is 20466mg/L, after flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 17217mg/L, and no BOD is detected.
EXAMPLE III
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 61.32g, the addition amount of 30% hydrogen peroxide solution is 181ML, the reaction is carried out for 2 hours, the obtained reaction mixed solution is sampled and detected, the COD content is 16223mg/L, after the flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 15157mg/L, the BOD content is 8460mg/L, and the BC ratio is 0.47.
Example four
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 81.76g, the addition amount of 30% hydrogen peroxide solution is 181ML, the reaction is carried out for 2 hours, the obtained reaction mixed solution is subjected to sampling detection, the COD content is 16343mg/L, after the flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 14368mg/L, the BOD content is 8220mg/L, and the BC ratio is 0.60.
EXAMPLE five
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 49.06g, the addition amount of epoxidation reaction wastewater is 272ML, the reaction is carried out for 2 hours, the obtained reaction mixed liquid is subjected to sampling detection, the COD content is 18067mg/L, after flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 15157mg/L, the BOD content is 8460mg/L, and the BC ratio is 0.30.
EXAMPLE six
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 61.32g, the addition amount of epoxidation reaction wastewater is 272ML, the reaction is carried out for 2 hours, the obtained reaction mixed liquid is sampled and detected, the COD content is 12000mg/L, after the flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 10150mg/L, the BOD content is 7136mg/L, and the BC ratio is 0.51.
EXAMPLE seven
In step S2, the total amount of wastewater in the first reaction tank is 300ML, the COD content is 94598mg/L, in step S3, the addition amount of FeSO4 & 7H2O is 81.76g, the addition amount of epoxidation reaction wastewater is 272ML, the reaction is carried out for 2 hours, the obtained reaction mixed liquid is subjected to sampling detection, the COD content is 10000mg/L, after the flocculation reaction is carried out in step S4, the supernatant is taken for sampling detection again, the COD content is 8733mg/L, the BOD content is 7681mg/L, and the BC ratio is 0.74.
The experimental data comparison of the 7 embodiments shows that the esterification wastewater treatment experimental method provided by the invention can effectively reduce the COD content of the esterification wastewater, can further reduce the COD content after flocculation reaction, and compared with the treatment of 30% hydrogen peroxide, when FeSO4 & 7H2O with the same amount is used for treatment, the epoxidation wastewater is added more, so that the COD content of the esterification wastewater can be better reduced, and the treatment of the epoxidation wastewater can be realized, thereby being beneficial to reducing the cost of subsequent wastewater treatment of enterprises, and achieving multiple purposes.
According to the esterification reaction wastewater treatment experimental method, when wastewater is treated, the wastewater of the esterification reaction and the wastewater of the epoxidation reaction are combined through the matching of all the steps, and the matching of a plurality of reaction solutions can effectively reduce the COD value of the wastewater of the esterification reaction and dilute the concentration of hydrogen peroxide in the wastewater of the epoxidation reaction, so that the simultaneous treatment of two kinds of wastewater is realized, the convenience is high, the B/C ratio of the wastewater is reduced, and the biochemical property of the wastewater is improved.
In the experiment, FeSO4 & 7H2O and hydrogen peroxide solution are firstly used for reacting the wastewater, and then the wastewater is flocculated by the reaction solution, so that the precipitation of substances generated by the reaction can be accelerated, and the COD value of the wastewater can be further reduced.
The wastewater of the esterification reaction and the wastewater of the epoxidation reaction are combined, and the wastewater of the epoxidation reaction contains hydrogen peroxide to treat the esterification wastewater, so that the raw material hydrogen peroxide for treating the esterification wastewater is saved, the PH of the wastewater is not required to be adjusted due to the organic acid contained in the wastewater of the epoxidation reaction, and the problem of additionally treating the wastewater of high-concentration hydrogen peroxide is solved.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. An esterification reaction wastewater treatment experimental method is characterized in that: comprises the following steps
S1: firstly, preparing reaction solution required by an experiment, wherein the reaction solution comprises 10% PAC solution, 2% o PAM solution and 10% NaOH solution;
s2: adding esterification wastewater in production of a bio-based plasticizer into a first reaction tank for waiting for treatment, and waiting epoxidation wastewater for standby application, wherein the esterification wastewater contains an esterified substance, alcohol and vegetable oleic acid, and the epoxidation wastewater contains 20% of hydrogen peroxide and organic acid;
s3: adding FeSO 4.7H 2O into the first reaction tank, dropwise adding epoxidation wastewater into the first reaction tank, uniformly stirring by using a glass rod, standing, and reacting for 2-4 hours to obtain a reaction mixed solution;
s4: dripping 10% NaOH solution into the first reaction tank, adjusting the pH value of the reaction mixed solution to 8-9, dripping 10% PAC solution and 2 thousandth PAM solution into the first reaction tank, performing flocculation reaction on the reaction mixed solution, and taking supernatant in the first reaction tank for subsequent treatment after the reaction is completely precipitated;
s5: after the reaction is finished, taking the supernatant into a second reaction tank, adding NaOH solution into the second reaction tank, adjusting the pH value of the supernatant back to 10 to remove iron ions in the supernatant, uniformly stirring, standing for precipitation, and taking the supernatant for detection of each index;
s6: and recording the experimental result, wherein the type of the added medicine, the dosage, the experimental process, the reaction and precipitation time, the sludge amount and the condition of the supernatant in the experimental process are recorded, and a picture of the experimental process is left.
2. The experimental method for treating esterification reaction wastewater according to claim 1, wherein: in the step S3, the addition amount of FeSO 4.7H 2O is 8-30% of the amount of the esterification reaction wastewater.
3. The experimental method for treating esterification reaction wastewater according to claim 1, wherein: in the step S3, the addition amount of the wastewater of the epoxidation reaction is 30-60% of the amount of the wastewater of the esterification reaction, and the addition speed of the wastewater of the epoxidation reaction is 150 kg/h-300 kg/h per ton of the wastewater.
4. The experimental method for treating esterification reaction wastewater according to claim 1, wherein: in the step S4, the dropping speed of the PAC solution is 0.05 kg/h-0.25 kg/h per ton of wastewater, and the dropping amount of the PAC solution is 0.1% -0.5% of the amount of the esterification reaction wastewater.
5. The experimental method for treating esterification reaction wastewater according to claim 1, wherein: in the step S4, the dropping speed of the PAM solution is 0.45 kg/h-1.25 kg/h per ton of wastewater, and the dropping amount of the PAM solution is 1% -3% of the amount of the esterification reaction wastewater.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3933630A (en) * | 1973-09-12 | 1976-01-20 | Rhone-Progil | Purification of waste water containing phthalic esters |
| CN101224937A (en) * | 2008-02-01 | 2008-07-23 | 浙江嘉澳化工有限公司 | Reuse treating method for chemical industrial plasticizer waste water |
| CN105254117A (en) * | 2015-09-24 | 2016-01-20 | 安庆丰源化工有限公司 | Treatment method of fine chemical engineering oily wastewater |
| CN106517670A (en) * | 2016-12-19 | 2017-03-22 | 天津凯英科技发展股份有限公司 | Advanced treatment technology for wastewater |
| CN108640433A (en) * | 2018-05-31 | 2018-10-12 | 张荣斌 | A kind of gelatin comprehensive effluent disposal technology |
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- 2021-07-29 CN CN202110864408.3A patent/CN113443750B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3933630A (en) * | 1973-09-12 | 1976-01-20 | Rhone-Progil | Purification of waste water containing phthalic esters |
| CN101224937A (en) * | 2008-02-01 | 2008-07-23 | 浙江嘉澳化工有限公司 | Reuse treating method for chemical industrial plasticizer waste water |
| CN105254117A (en) * | 2015-09-24 | 2016-01-20 | 安庆丰源化工有限公司 | Treatment method of fine chemical engineering oily wastewater |
| CN106517670A (en) * | 2016-12-19 | 2017-03-22 | 天津凯英科技发展股份有限公司 | Advanced treatment technology for wastewater |
| CN108640433A (en) * | 2018-05-31 | 2018-10-12 | 张荣斌 | A kind of gelatin comprehensive effluent disposal technology |
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