CN111747435A - Method for preparing flocculant by using oxadiargyl byproduct - Google Patents
Method for preparing flocculant by using oxadiargyl byproduct Download PDFInfo
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- CN111747435A CN111747435A CN202010650682.6A CN202010650682A CN111747435A CN 111747435 A CN111747435 A CN 111747435A CN 202010650682 A CN202010650682 A CN 202010650682A CN 111747435 A CN111747435 A CN 111747435A
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- Prior art keywords
- flocculant
- solution
- acidity
- oxadiargyl
- stock solution
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- Granted
Links
- 239000006227 byproduct Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 31
- DVOODWOZJVJKQR-UHFFFAOYSA-N 5-tert-butyl-3-(2,4-dichloro-5-prop-2-ynoxyphenyl)-1,3,4-oxadiazol-2-one Chemical group O=C1OC(C(C)(C)C)=NN1C1=CC(OCC#C)=C(Cl)C=C1Cl DVOODWOZJVJKQR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 94
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 63
- 239000011550 stock solution Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 17
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 17
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000012797 qualification Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 9
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 5
- 238000004448 titration Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 238000006266 etherification reaction Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 239000012085 test solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011592 zinc chloride Substances 0.000 description 4
- 235000005074 zinc chloride Nutrition 0.000 description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000006193 diazotization reaction Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 239000008394 flocculating agent Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000007363 ring formation reaction Methods 0.000 description 3
- 239000001119 stannous chloride Substances 0.000 description 3
- 235000011150 stannous chloride Nutrition 0.000 description 3
- HFZWRUODUSTPEG-UHFFFAOYSA-N 2,4-dichlorophenol Chemical compound OC1=CC=C(Cl)C=C1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QUIMTLZDMCNYGY-UHFFFAOYSA-N 2,4-dichloro-1-nitrobenzene Chemical group [O-][N+](=O)C1=CC=C(Cl)C=C1Cl QUIMTLZDMCNYGY-UHFFFAOYSA-N 0.000 description 1
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N N-phenyl amine Natural products NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 125000002490 anilino group Chemical class [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- LJZPPWWHKPGCHS-UHFFFAOYSA-N propargyl chloride Chemical compound ClCC#C LJZPPWWHKPGCHS-UHFFFAOYSA-N 0.000 description 1
- 238000006462 rearrangement reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical compound C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- 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
- C02F1/52—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
Abstract
The application provides a method for preparing a flocculant by using oxadiargyl by-products, which comprises the following steps: detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%; adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution; reacting the reaction solution at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution; and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant. The method for preparing the flocculant by using the oxadiargyl by-product is based on the prior art, and is used for further treating the polyaluminium chloride generated in the production, so that the content of the polyaluminium chloride is more than or equal to 10 percent and reaches the national standard of the qualification of the polyaluminium chloride, thereby realizing the recycling of the by-product of the oxadiargyl process, improving the efficiency, saving energy and reducing emission.
Description
Technical Field
The application relates to the technical field of flocculating agents, in particular to a method for preparing a flocculating agent by using oxadiargyl byproducts.
Background
The first method is to adopt 2, 4-dichlorophenol as an initial raw material and carry out the steps of nitration, etherification, reduction, diazotization, acidification, cyclization and the like; secondly, 2, 4-dichlorophenol is used as an initial raw material, an intermediate substituted aniline is prepared through etherification, nitration and reduction, phthalylation is carried out, and finally, the target compound is obtained through cyclization with phosgene; the third is 2, 4-dichloronitrobenzene, 5-tert-butyl-1, 3, 4-oxadiazole-2 (3H) -ketone as the starting material, and the target product is obtained through coupling, reduction and rearrangement reaction and final etherification with propargyl chloride.
In the process of preparing oxadiargyl, byproduct polyaluminium chloride is generated, the polyaluminium chloride can be sold and used as a flocculating agent, but the content of the aluminum chloride generated in the process is between 5 and 6 percent and does not meet the national standard. Many plants require specialized companies to handle this portion of the by-product, increasing production costs. So the polyaluminium chloride which is the byproduct of oxadiargyl is difficult to recycle at present.
Disclosure of Invention
The application provides a method for preparing a flocculant by using an oxadiargyl byproduct, which aims to solve the problem that polyaluminium chloride as the oxadiargyl byproduct is difficult to recycle.
The application provides a method for preparing a flocculant by using oxadiargyl byproducts, which comprises the following steps:
detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%;
adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution;
reacting the reaction solution at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution;
and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant.
Optionally, the acidity of the polyaluminium chloride solution is detected and adjusted, so that the acidity of the polyaluminium chloride solution is adjusted in a step of 15-20%, the acidity of the polyaluminium chloride solution is adjusted by using caustic soda flakes or hydrogen chloride gas, and the acidity of the polyaluminium chloride solution is higher than 15-20% and is adjusted by using caustic soda flakes; and regulating the acidity of the polyaluminium chloride solution by using hydrogen chloride gas when the acidity is lower than 15-20%.
Optionally, in the step of adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain the reaction solution, the mass ratio of the polyaluminium chloride solution to the added calcium aluminate and sodium thiosulfate is 75 (8-12): 2.
Optionally, in the step of reacting the reaction solution at 80-100 ℃ for 3-5h and cooling to room temperature to obtain the flocculant stock solution, standing the obtained flocculant stock solution at room temperature for 24-36 h.
Optionally, the acidity of the flocculant stock solution is detected and adjusted to be 10-13%, and in the step of obtaining the flocculant, the acidity of the flocculant stock solution is adjusted by using caustic soda flakes.
Optionally, the mass fraction of the alumina in the obtained flocculant is more than or equal to 10%.
According to the technical scheme, the method for preparing the flocculant by using the oxadiargyl byproduct provided by the application comprises the following steps: the application provides a method for preparing a flocculant by using oxadiargyl by-products, which comprises the following steps: detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%; adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution; reacting the reaction solution at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution; and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant. The method for preparing the flocculant by using the oxadiargyl by-product is based on the prior art, and is used for further treating the polyaluminium chloride generated in the production, so that the content of the polyaluminium chloride is more than or equal to 10 percent and reaches the national standard of the qualified polyaluminium chloride, thereby realizing the recycling of the by-product of the oxadiargyl process, improving the efficiency, saving energy and reducing emission.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a process for preparing a flocculant from oxadiargyl by-product according to an embodiment of the present application.
Detailed Description
Reference will now be made in detail to embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following examples do not represent all embodiments consistent with the present application. But merely as exemplifications of systems and methods consistent with certain aspects of the application, as recited in the claims.
The process flow for preparing oxadiargyl comprises the following steps: esterification, etherification, diazotization, cyclization, hydrolysis and synthesis. During the diazotization process, a centrifugal mother liquor is used for removing a reducing agent stannous chloride and recovering the working section. The recovery of the reducing agent stannous chloride is to recover elemental tin which is generated by reduction reaction of stannic chloride which is generated by reaction and incompletely reacted stannous chloride in the original system. In the process, aluminum powder is used as a reducing agent for reducing tin ions, and finally tin simple substances are recovered through suction filtration, so that mother liquor becomes a byproduct flocculant, but in the production process, the content of effective component alumina in the byproduct flocculant cannot reach the product index of the national standard due to the influence of material proportion and related factors, so that the flocculant needs to be further processed to reach the national standard, the byproduct flocculant can be sold, the flocculant is distilled and concentrated to reach the standard, and the production cost is higher than the sales profit.
The application provides a method for preparing a flocculant by using oxadiargyl byproducts, which comprises the following steps:
s1: detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%;
performing acidity test on a polyaluminium chloride solution, namely initial mother liquor, and performing acidity adjustment on the mother liquor by using caustic soda flakes or hydrogen chloride gas to control the acidity of the mother liquor to be 15-20%;
wherein the acidity of the polyaluminium chloride solution is higher than 15-20% and the acidity is adjusted by using caustic soda flakes; and regulating the acidity of the polyaluminium chloride solution by using hydrogen chloride gas when the acidity is lower than 15-20%.
In practical application, since the addition of alkaline solution or acidic solution can affect the purity and basicity of the solution and bring in additional impurities, when the polyaluminium chloride solution is adjusted, alkaline solid flake alkali or hydrogen chloride gas is adopted, so that the damage to the basicity of the solution and the influence on the purity of the solution can be avoided.
S2: adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution;
and adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution, wherein the mass ratio of the polyaluminium chloride solution to the added calcium aluminate and sodium thiosulfate is 75 (8-12) to 2, and the step is carried out at normal temperature.
In practical applications, sodium thiosulfate is used as an antioxidant to prevent oxidation due to elevated temperatures in the subsequent step.
S3: reacting the reaction solution at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution;
reacting the polyaluminium chloride solution added with calcium aluminate and sodium thiosulfate at 80-100 ℃ for 3-5h, cooling to room temperature to obtain a flocculant stock solution, and standing the flocculant stock solution at room temperature for 24-36 h.
The reaction equation for the participation of calcium aluminate during the high temperature reaction is shown below:
CaO.Al2O3+3HCl＝Al2(OH)nCl6-n+CaCl2+2H2O；
the reaction is carried out to a certain degree, and when the pH value is proper, two adjacent hydroxyl groups of the aluminum chloride generate bridging action to polymerize and self-polymerize, and are finally converted into polyaluminium chloride, and the specific reaction is as follows:
mAl2(OH)nCl6-n＝[Al2(OH)nCl6-n]m；
in practical application, the flocculant stock solution obtained is kept stand at room temperature for 24-36h because precipitation is generated in the step, the obtained stock solution is difficult to filter, and the flocculant stock solution obtained is kept stand at room temperature for 24-36h in order to settle the precipitation.
S4: and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant.
In practical application, the flocculant stock solution obtained in the previous step S3 needs to be filtered, the acidity of the flocculant stock solution after filtering is detected after impurities are removed, and the acidity of the flocculant stock solution is adjusted by using caustic soda flakes, so that the acidity of the flocculant stock solution is controlled to be 10-13%, and finally the flocculant is obtained. The mass fraction of the alumina in the flocculant is improved from 5-6% to 10-15% by the method for preparing the flocculant. Fig. 1 is a schematic flow chart of a process for preparing a flocculant from oxadiargyl by-product according to an embodiment of the present application.
Wherein the content of alumina in the flocculant is analyzed and calculated by the following steps:
weighing 13g of the flocculant liquid sample, dissolving the flocculant liquid sample with ultrapure water to obtain a solution, transferring the solution into a 250mL volumetric flask, diluting to a scale, and shaking up. Dry-filter with medium speed filter paper and label the solution as test solution a.
Weighing 10mL of test solution A, placing the test solution A in a 250mL conical flask, adding 10mL of nitric acid solution, boiling for 1min, cooling to room temperature, adding 20mL of ethylene diamine tetraacetic acid disodium solution, dropwise adding 3 drops of thymol blue indicator solution, neutralizing with ammonia water solution until the test solution turns from red to yellow, and boiling for 2 min. After cooling, 10mL of acetic acid-sodium acetate buffer solution and two drops of xylenol orange indicator solution are added, 50mL of water is added, zinc chloride standard titration solution is used for titration until the solution changes from light yellow to reddish, namely, a midpoint, and meanwhile, a blank experiment is carried out.
The content of alumina is in mass fraction omega1In% by weight, the value is calculated as follows:
V0the value of the volume of the standard titration solution of zinc chloride consumed for the blank test, V the value of the volume of the standard titration solution of zinc chloride consumed for the test sample, c the value of the actual concentration of the standard titration solution of zinc chloride, M the molar mass of aluminum chloride, M the mass of the test sample, V1Value of volume of the sample solution A, VAIs a value of the total volume of the sample solution A.
The following is a first embodiment provided by the present application:
300mL of polyaluminum chloride solution with an alumina content of 5.88% was placed in a beaker. The polyaluminum chloride solution was subjected to an acidity test, and the acidity of the solution was adjusted to 20% using caustic soda flakes.
The above polyaluminum chloride solution was transferred to a four-necked flask, 43g of calcium aluminate and 10g of sodium thiosulfate were added to the solution at normal temperature, and a thermometer, a condenser and a stirrer were provided to the four-necked flask. The electric stirrer was turned on and the solution was stirred until the solid was completely dissolved. The stirring device used therein is a tetrafluoro stir bar because of its acid and alkali resistance.
And (3) moving the four-mouth flask into an electric heating jacket for heating, stirring and heating at the moment, stopping heating when the temperature reaches 80 ℃, performing condensation reflux by using a condensing tube, reacting for 2 hours, heating to 90 ℃, reacting for 2 hours, finishing the reaction, and cooling the obtained flocculant stock solution to room temperature.
And standing the flocculant stock solution at room temperature for 36 hours, performing suction filtration on the flocculant stock solution by using a vacuum pump, removing impurities to obtain a solution, namely the flocculant stock solution, performing acidity test on the flocculant stock solution, adding 15g of flake caustic soda to control the acidity of the flocculant stock solution to be 10%, and finally obtaining the flocculant. Wherein the content of the aluminum oxide in the flocculant is 10.25 percent. The mass fraction of water insoluble substances in the flocculant is less than or equal to 0.4 percent, the mass fraction of Fe is less than or equal to 3.5 percent, the mass fraction of As is less than or equal to 0.0005 percent, the mass fraction of Pb is less than or equal to 0.002 percent, the mass fraction of Cd is less than or equal to 0.01 percent, the mass fraction of Hg is less than or equal to 0.00005 percent, and the mass fraction of Cr is less than or equal to 0.05.
The following is a second example provided by the present application:
300ml of polyaluminium chloride solution is taken in a beaker, wherein the content of alumina in the polyaluminium chloride solution is 5.76 percent. The polyaluminum chloride solution was subjected to an acidity test, and the acidity of the solution was adjusted to 15% using caustic soda flakes.
The above polyaluminum chloride solution was transferred to a four-necked flask, 40g of calcium aluminate and 10g of sodium thiosulfate were added to the solution at normal temperature, and a thermometer, a condenser and a stirrer were provided to the four-necked flask. The electric stirrer was turned on and the solution was stirred until the solid was completely dissolved. The stirring device used therein is a tetrafluoro stir bar because of its acid and alkali resistance.
And (3) moving the four-mouth flask into an electric heating jacket for heating, stirring and heating at the moment, stopping heating when the temperature reaches 90 ℃, performing condensation reflux by using a condensing tube, reacting for 2 hours, heating to 100 ℃, reacting for 1 hour, and finishing the reaction to obtain a flocculant stock solution and cooling to room temperature.
And standing the flocculant stock solution at room temperature for 24 hours, performing suction filtration on the flocculant stock solution by using a vacuum pump, removing impurities to obtain a solution, namely the flocculant stock solution, performing acidity test on the flocculant stock solution, adding 13g of flake caustic soda to control the acidity of the flocculant stock solution to be 13%, and finally obtaining the flocculant. Wherein the content of the aluminum oxide in the flocculant is 10.13 percent. The mass fraction of water insoluble substances in the flocculant is less than or equal to 0.4%, the mass fraction of Fe is less than or equal to 3.5%, the mass fraction of As is less than or equal to 0.0005%, the mass fraction of Pb is less than or equal to 0.002%, the mass fraction of Cd is less than or equal to 0.01%, the mass fraction of Hg is less than or equal to 0.00005%, and the mass fraction of Cr is less than or equal to 0.05%.
The following is a third embodiment provided by the present application:
300ml of polyaluminium chloride solution is taken in a beaker, wherein the content of alumina in the polyaluminium chloride solution is 5.52 percent. The polyaluminum chloride solution was subjected to an acidity test, and the acidity of the solution was adjusted to 18% using caustic soda flakes.
The above polyaluminum chloride solution was transferred to a four-necked flask, 40g of calcium aluminate and 10g of sodium thiosulfate were added to the solution at normal temperature, and a thermometer, a condenser and a stirrer were provided to the four-necked flask. The electric stirrer was turned on and the solution was stirred until the solid was completely dissolved. The stirring device used therein is a tetrafluoro stir bar because of its acid and alkali resistance.
And (3) moving the four-mouth flask into an electric heating jacket for heating, stirring and heating at the moment, stopping heating when the temperature reaches 90 ℃, performing condensation reflux by using a condensing tube, reacting for 2 hours, heating to 100 ℃, reacting for 3 hours, and finishing the reaction to obtain a flocculant stock solution and cooling to room temperature.
And standing the flocculant stock solution at room temperature for 36 hours, performing suction filtration on the flocculant stock solution by using a vacuum pump, removing impurities to obtain a solution, namely the flocculant stock solution, performing acidity test on the flocculant stock solution, adding 13.5g of flake caustic soda to control the acidity of the flocculant stock solution to be 11%, and finally obtaining the flocculant. Wherein the content of alumina in the flocculant is 11%. The mass fraction of water insoluble substances in the flocculant is less than or equal to 0.4 percent, the mass fraction of Fe is less than or equal to 3.5 percent, the mass fraction of As is less than or equal to 0.0005 percent, the mass fraction of Pb is less than or equal to 0.002 percent, the mass fraction of Cd is less than or equal to 0.01 percent, the mass fraction of Hg is less than or equal to 0.00005 percent, and the mass fraction of Cr is less than or equal to 0.05.
According to the technical scheme, the method for preparing the flocculant by using the oxadiargyl byproduct provided by the application comprises the following steps: the application provides a method for preparing a flocculant by using oxadiargyl by-products, which comprises the following steps: detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%; adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution; reacting the reaction liquid at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution; and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant. The method for preparing the flocculant by using the oxadiargyl by-product is based on the prior art, and is used for further treating the polyaluminium chloride generated in the production, so that the content of the polyaluminium chloride is more than or equal to 10 percent and reaches the national standard of the qualification of the polyaluminium chloride, thereby realizing the recycling of the by-product of the oxadiargyl process, improving the efficiency, saving energy and reducing emission.
Claims (6)
1. A method for preparing a flocculant by using oxadiargyl by-product is characterized by comprising the following steps:
detecting and adjusting the acidity of the polyaluminium chloride solution to enable the acidity of the polyaluminium chloride solution to be 15-20%;
adding calcium aluminate and sodium thiosulfate into the polyaluminium chloride solution to obtain a reaction solution;
reacting the reaction solution at 80-100 ℃ for 3-5h, and cooling to room temperature to obtain a flocculant stock solution;
and detecting and adjusting the acidity of the flocculant stock solution to enable the acidity of the flocculant stock solution to be 10-13% to obtain the flocculant.
2. The method for preparing the flocculant by using the oxadiargyl by-product as the claim 1, wherein the acidity of the polyaluminum chloride solution is detected and adjusted to be 15-20%, the acidity of the polyaluminum chloride solution is adjusted by using caustic soda flakes or hydrogen chloride gas, and the acidity of the polyaluminum chloride solution is higher than 15-20% and is adjusted by using caustic soda flakes; and regulating the acidity of the polyaluminium chloride solution by using hydrogen chloride gas when the acidity is lower than 15-20%.
3. The method for preparing the flocculant by using the oxadiargyl by-product according to claim 1, wherein in the step of adding calcium aluminate and sodium thiosulfate into the polyaluminum chloride solution to obtain the reaction solution, the mass ratio of the polyaluminum chloride solution to the added calcium aluminate and sodium thiosulfate is 75 (8-12): 2.
4. The method for preparing the flocculant by using the oxadiargyl by-product as claimed in claim 1, wherein in the step of reacting the reaction solution at 80-100 ℃ for 3-5h and cooling to room temperature to obtain the flocculant stock solution, the obtained flocculant stock solution is allowed to stand at room temperature for 24-36 h.
5. The method for preparing the flocculant by using the oxadiargyl by-product as claimed in claim 1, wherein the step of detecting and adjusting the acidity of the flocculant stock solution to make the acidity of the flocculant stock solution be 10-13%, and the step of adjusting the acidity of the flocculant stock solution in the step of obtaining the flocculant, is performed by using caustic soda flakes.
6. The method for preparing the flocculant by using the oxadiargyl by-product according to claim 1, wherein the mass fraction of alumina in the obtained flocculant is more than or equal to 10%.
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Denomination of invention: A method for preparing flocculants using byproducts of propargyl oxalate Granted publication date: 20221025 Pledgee: China Postal Savings Bank Co.,Ltd. Shizuishan Branch Pledgor: Ningxia Lantian Agricultural Development Co.,Ltd. Registration number: Y2024980010645 |
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