CN115181222B - Preparation method of organic polymeric flocculant for water treatment - Google Patents
Preparation method of organic polymeric flocculant for water treatment Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 8
- GNOZLGOOOBMHRC-UHFFFAOYSA-L iron(2+);prop-2-enoate Chemical compound [Fe+2].[O-]C(=O)C=C.[O-]C(=O)C=C GNOZLGOOOBMHRC-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 8
- SAXJVKAVLPPFLI-UHFFFAOYSA-N prop-2-enoic acid;1,1,3,3-tetramethylguanidine Chemical compound OC(=O)C=C.CN(C)C(=N)N(C)C SAXJVKAVLPPFLI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000003396 thiol group Chemical group [H]S* 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000003999 initiator Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 12
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 12
- 229920000620 organic polymer Polymers 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 210000003298 dental enamel Anatomy 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002245 particle Substances 0.000 abstract description 7
- 238000005189 flocculation Methods 0.000 abstract description 6
- 230000016615 flocculation Effects 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000007259 addition reaction Methods 0.000 abstract description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract description 2
- 239000002332 oil field water Substances 0.000 abstract description 2
- -1 acrylic ester Chemical class 0.000 abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 31
- 239000007788 liquid Substances 0.000 description 26
- 238000009833 condensation Methods 0.000 description 15
- 230000005494 condensation Effects 0.000 description 15
- 239000003921 oil Substances 0.000 description 15
- 230000003647 oxidation Effects 0.000 description 15
- 238000007254 oxidation reaction Methods 0.000 description 15
- 239000002351 wastewater Substances 0.000 description 14
- 238000001035 drying Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 10
- 238000007599 discharging Methods 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 10
- 238000004064 recycling Methods 0.000 description 10
- 238000007670 refining Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 229940035049 sorbitan monooleate Drugs 0.000 description 6
- 235000011069 sorbitan monooleate Nutrition 0.000 description 6
- 239000001593 sorbitan monooleate Substances 0.000 description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 5
- MWFMGBPGAXYFAR-UHFFFAOYSA-N 2-hydroxy-2-methylpropanenitrile Chemical compound CC(C)(O)C#N MWFMGBPGAXYFAR-UHFFFAOYSA-N 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002192 fatty aldehydes Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to the field of chemical industry, in particular to a preparation method of an organic polymeric flocculant for water treatment; the method comprises the steps of carrying out addition reaction on iron acrylate and sulfhydryl polyethylene glycol acrylic ester to obtain iron-containing polyethylene glycol acrylic ester, and carrying out copolymerization reaction on the iron-containing polyethylene glycol acrylic ester, tetramethylguanidine acrylate, acrylamide and vinylguanamine to obtain the organic polymeric flocculant; the function principle is that active sites contained in a molecular chain and suspended particles generate chemical adsorption bridging action to form floccules of a colloidal particle flocculant-colloidal particle structure, so that the size of the floccules is increased; the organic flocculant can improve the flocculation effect through the effects of electric neutralization and adsorption bridging, so that the flocculant has the characteristics of low dosage, quick sedimentation and good flocculation effect in oilfield water treatment, and is beneficial to quick sedimentation and removal of pollutants; solves the problems of low efficiency, high consumption, secondary pollution and the like of the common flocculant.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of an organic polymeric flocculant for water treatment.
Background
Because of exploiting the low permeability oil field, it is difficult to effectively improve the quality of the reinjection water, the pollutant liquid discharged into the environment is gradually increased, the flocculant is used as an important water treatment agent, the research and development of the high-efficiency low-consumption safe harmless organic flocculant has become a hotspot in the research field of domestic and foreign flocculants, and the flocculants for treating the oily wastewater in the oil field are as follows: inorganic flocculant, organic flocculant and composite flocculant.
CN01127795.5: the invention relates to an organic polymer flocculant, a preparation method and application thereof in water treatment, wherein the preparation method comprises the steps of carrying out polycondensation reaction, dissolving inorganic ammonium salt in a reactor containing fatty aldehyde and water, wherein the reaction temperature is 10-60 ℃, adding dicyandiamide, and controlling the reaction temperature to 60-95 ℃ and the reaction time to 0.5-3 hours; the hydrolysis reaction and the esterification reaction, the temperature of the reaction liquid is reduced to 20-70 ℃, phosphorus trichloride is added, the reaction temperature is increased to 90-120 ℃, the reaction is carried out for 2-9 hours, the temperature of the materials is reduced to 45-85 ℃, additives are added, the reaction is continued for 1-3 hours, and the product is obtained after cooling to room temperature; the product has ideal wastewater treatment effect, good product stability, no toxicity, no limitation of seasons and areas, and convenient storage and transportation.
CN201510590969.3: in the organic polymeric flocculant for polymer-containing sewage treatment and the preparation method thereof, the components before mixing reaction are as follows by mass fraction: 30-40% of polyaluminum chloride, wherein the mass of the nonionic polyacrylamide is 5% of that of the polyaluminum chloride; the mass ratio of the polydimethyl diallyl ammonium chloride to the polyaluminum chloride is 1-2:2-3. The weak cation type organic polymer flocculant obtained after the polymerization reaction has extremely strong flocculation effect, effectively removes organic impurities and emulsified oil in the waste water containing the polymerized crude oil, and has less quality and stable form of the produced floccules; the invention is prepared by adopting a compound method, and has the advantages of simple process, readily available raw materials, no toxic or side effect, high efficiency of water purification effect, low cost, small usage amount and the like.
CN201811406558.4: the invention discloses an organic polymeric flocculant and a preparation method and application thereof, wherein the flocculant is formed by wrapping nano zero-valent iron with an organic polymeric flocculant, has uniform particle size distribution, has a dispersed uniform spherical particle shape, is prepared by mixing and stirring the nano zero-valent iron and the organic polymeric flocculant by using absolute ethyl alcohol as a protective agent in a nitrogen environment, then dripping a reducing agent solution, stirring after dripping, enabling the organic polymeric flocculant to fully wrap the nano zero-valent iron, standing and aging, filtering to obtain black precipitate, cleaning, drying and storing. The invention combines the nano zero-valent iron and the organic polymeric flocculant, and the obtained modified zero-valent nano iron has good dispersibility and is not easy to agglomerate. The method is applied to sewage and sludge treatment, and has good effect of removing organic pollutants and heavy metals. The method is simple and easy to implement, has obvious modification effect, has good treatment effect on sewage and sludge, and reduces the pollution influence on the environment.
The above patents and the prior art, wherein the inorganic flocculant and the composite flocculant are proved to have large usage amount and poor flocculation effect on fine particles; and the organic polymeric flocculant has the defects of low oil removal rate in the wastewater and the like.
Disclosure of Invention
In order to solve the problems, the first technical scheme adopted by the invention is as follows:
the preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: according to the weight portions, 10 to 15 portions of acrylic acid and 17 to 28 portions of tetramethylguanidine are heated, the temperature is raised, the mixture is sealed and strongly stirred mechanically for 3 to 5 hours to obtain the tetramethylguanidine acrylate,
s2: fully dissolving 1-5 parts of span80 in 50-100 parts of cyclohexane solution, adding 20-30 parts of acrylamide, 0.2-2 parts of vinylguanamine and 7-12 parts of synergist into a reactor, stirring and heating;
s3: adding 2-6 parts of initiator into the acrylic acid solution after S1 neutralization, and stirring to obtain an organic polymer flocculant;
in the first embodiment, preferably, the heating temperature in S1 is 40 to 50 ℃.
In the first technical scheme, preferably, the S2 is continuously introduced with nitrogen for 0.5-2h.
In a first embodiment, preferably, the span80 is sorbitan monooleate.
In the first aspect, preferably, the stirring rate is 500 to 600 rpm.
In the first embodiment, preferably, the reaction temperature of S2 is 45 to 60 ℃.
In the first embodiment, preferably, the reactor is made of plastic, enamel, aluminum or stainless steel.
The second technical scheme adopted by the invention is as follows: the preparation method of the synergist comprises the following steps:
according to the weight portions, 10-15 portions of iron acrylate, 5-12 portions of sulfhydryl polyethylene glycol acrylate, 50-100 portions of cyclohexane solution, 3-7 portions of triethylamine are added into a reaction kettle, and the temperature is raised and nitrogen is continuously introduced for 1-3 hours, thus obtaining the synergist.
In the second embodiment, the reaction temperature is preferably 60 to 70 ℃.
The third technical scheme adopted by the invention is as follows: the preparation method of the initiator comprises the following steps:
s1 (condensation, oxidation): adding the oxidation circulating liquid, 4-6 parts of hydrazine hydrate and 10-15 parts of acetone cyanohydrin into a condensation kettle, stirring, and reacting at 25-50 ℃; after 2h, cl2 is introduced into the kettle through a Cl2 distributor, and after Cl2 2-3h, discharging is carried out; filtering, washing and spin-drying to obtain Cl2 material (i.e. crude azodiisobutyronitrile product); recovering waste liquid (called circulating liquid) and returning to the condensation section;
s2 (refining): oxidizing material: ethanol is prepared according to the following proportion of 1:1.1 to 1.2, putting the mixture into a refining kettle, and obtaining an azo-diisobutyronitrile initiator through dissolution, crystallization, discharging, spin-drying and vacuum drying; recovering mother liquor, distilling to obtain ethanol, and recycling; and recovering distillation residual liquid (circulating liquid), and returning to the oxidation section for recycling.
The core technology of the invention is as follows:
and (3) performing addition reaction on the iron acrylate and the sulfhydryl polyethylene glycol acrylate to obtain iron-containing polyethylene glycol acrylate, and performing copolymerization reaction on the iron-containing polyethylene glycol acrylate, the tetramethylguanidine acrylate, the acrylamide and the vinylguanamine to obtain the organic polymeric flocculant.
The beneficial effects of using the invention are as follows:
compared with the prior art, the invention has the advantages that: the organic polymer flocculant prepared by the invention is floccule with a colloidal particle flocculant-colloidal particle structure through the chemical adsorption bridging effect of active sites contained in a molecular chain and suspended matter particles, so that the size of the floccule is increased; the organic flocculant macromolecular chains are also distributed with cations, anions or nonionic groups, and the cations, anions or nonionic groups are distributed on the macromolecular chains, so that the flocculation effect is improved through the electric neutralization and adsorption bridging effect, and the flocculant has the characteristics of low dosage, rapid sedimentation and good flocculation effect in oilfield water treatment, and is beneficial to rapid sedimentation and removal of pollutants; and solves the problems of low oil removal rate in the wastewater, and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present technical solution more clear, the present technical solution is further described in detail below in conjunction with specific embodiments and comparative examples. It should be understood that the description is only illustrative and is not intended to limit the scope of the present technical solution.
The calculation formula of the mass concentration of oil in the wastewater sample is as follows:
C＝m×1000/V
in the above formula, m is the amount of the corresponding oil detected from a standard curve, and the unit is mg; v is the volume of the water sample, and the unit is mL; c is the mass concentration of oil in the wastewater sample, and the unit is mg/L.
The calculation formula of the removal rate is as follows:
removal rate= (1-C/c.) x 100%
In the above formula, C. And C is the mass concentration of the wastewater sample before and after treatment, and the unit is mg/L.
Example 1
The preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: 10g of acrylic acid and 17g of tetramethylguanidine are heated, the temperature is raised, the mixture is stirred for 3 hours in a sealing and strong mechanical way, the tetramethylguanidine acrylate is obtained,
s2: 1g span80 is fully dissolved in 50g cyclohexane solution, 20g acrylamide, 0.2g vinylguanamine and 7g synergist are added into a reactor, and the mixture is stirred and heated;
s3: adding 2g of prepared S2 solution and 2g of initiator into the acrylic acid solution after S1 neutralization, and stirring to obtain an organic polymeric flocculant;
the heating temperature in S1 is 40 ℃.
And S2 is required to be continuously introduced with nitrogen for 0.5h.
The span80 is sorbitan monooleate.
The stirring rate was 500 rpm.
The reaction temperature of S2 is 45 ℃.
The reactor is made of plastic.
The preparation method of the synergist comprises the following steps:
10g of iron acrylate, 5g of sulfhydryl polyethylene glycol acrylate, 50g of cyclohexane solution, 3g of triethylamine are added into a reaction kettle, the temperature is raised, and nitrogen is continuously introduced for 1h, so as to obtain the synergist.
The reaction temperature was 60 ℃.
The preparation method of the initiator comprises the following steps:
s1 (condensation, oxidation): adding the oxidation circulating liquid, 4g of hydrazine hydrate and 10g of acetone cyanohydrin into a condensation kettle, stirring, and reacting at 25 ℃; after 2h, cl2 is introduced into the kettle through a Cl2 distributor, and after Cl2 2h, discharging is carried out; filtering, washing and spin-drying to obtain Cl2 material (i.e. crude azodiisobutyronitrile product); recovering waste liquid (called circulating liquid) and returning to the condensation section;
s2 (refining): oxidizing material: ethanol is prepared according to the following proportion of 1:1.1, putting the mixture into a refining kettle, and obtaining an azodiisobutyronitrile initiator through dissolution, crystallization, discharging, spin-drying and vacuum drying; recovering mother liquor, distilling to obtain ethanol, and recycling; and recovering distillation residual liquid (circulating liquid), and returning to the oxidation section for recycling.
The organic polymeric flocculant prepared by the experiment has the oil removal rate of 86.3 percent in wastewater.
Example 2
The preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: 12g of acrylic acid and 20g of tetramethylguanidine are heated, the temperature is raised, the mixture is sealed and strongly stirred for 3.5 hours by mechanical stirring, the tetramethylguanidine acrylate is obtained,
s2: 2g span80 is fully dissolved in 60g cyclohexane solution, 24g acrylamide, 1g vinylguanamine and 9g synergist are added into a reactor, and the mixture is stirred and heated;
s3: adding 3g of initiator into the prepared S2 solution in the acrylic acid solution after the neutralization of the S1, and stirring to obtain an organic polymeric flocculant;
the heating temperature in S1 was 44 ℃.
And S2, continuously introducing nitrogen for 1h.
The span80 is sorbitan monooleate.
The stirring rate was 540 revolutions per minute.
The reaction temperature of S2 is 50 ℃.
The reactor is made of enamel.
The preparation method of the synergist comprises the following steps:
12g of iron acrylate, 7g of sulfhydryl polyethylene glycol acrylate, 60g of cyclohexane solution, 4g of triethylamine are added into a reaction kettle, the temperature is raised, and nitrogen is continuously introduced for 1.5 hours, so as to obtain the synergist.
The reaction temperature was 64 ℃.
The preparation method of the initiator comprises the following steps:
s1 (condensation, oxidation): adding the oxidation circulating liquid, 5g of hydrazine hydrate and 12g of acetone cyanohydrin into a condensation kettle, stirring, and reacting at 30 ℃; after 2h, cl2 is introduced into the kettle through a Cl2 distributor, and after 2.5h of Cl2 is introduced, discharging is carried out; filtering, washing and spin-drying to obtain Cl2 material (i.e. crude azodiisobutyronitrile product); recovering waste liquid (called circulating liquid) and returning to the condensation section;
s2 (refining): oxidizing material: ethanol is prepared according to the following proportion of 1:1.1, putting the mixture into a refining kettle, and obtaining an azodiisobutyronitrile initiator through dissolution, crystallization, discharging, spin-drying and vacuum drying; recovering mother liquor, distilling to obtain ethanol, and recycling; and recovering distillation residual liquid (circulating liquid), and returning to the oxidation section for recycling.
The organic polymeric flocculant prepared by the experiment has the oil removal rate of 88.5 percent in wastewater.
Example 3
The preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: 14g of acrylic acid and 26g of tetramethylguanidine are heated, the temperature is raised, the mixture is stirred for 4 hours in a sealing and strong mechanical way, the tetramethylguanidine acrylate is obtained,
s2: 4g span80 is fully dissolved in 90g cyclohexane solution, 28g acrylamide, 1.5g vinylguanamine and 10g synergist are added into a reactor, and the mixture is stirred and heated;
s3: adding 5g of prepared S2 solution and 5g of initiator into the acrylic acid solution after the neutralization of the S1, and stirring to obtain an organic polymeric flocculant;
the heating temperature in S1 is 48 ℃.
And the S2 is required to be continuously introduced with nitrogen for 1.5 hours.
The span80 is sorbitan monooleate.
The stirring rate was 580 revolutions per minute.
The reaction temperature of S2 is 55 ℃.
The reactor is made of aluminum.
The preparation method of the synergist comprises the following steps:
14g of iron acrylate, 10g of sulfhydryl polyethylene glycol acrylate, 90g of cyclohexane solution, 6g of triethylamine are added into a reaction kettle, the temperature is raised, and nitrogen is continuously introduced for 2.5 hours, so as to obtain the synergist.
The reaction temperature was 68 ℃.
The preparation method of the initiator comprises the following steps:
s1 (condensation, oxidation): adding the oxidation circulating liquid, 5g of hydrazine hydrate and 14g of acetone cyanohydrin into a condensation kettle, stirring, and reacting at 45 ℃; after 2h, cl2 is introduced into the kettle through a Cl2 distributor, and after 2.5h of Cl2 is introduced, discharging is carried out; filtering, washing and spin-drying to obtain Cl2 material (i.e. crude azodiisobutyronitrile product); recovering waste liquid (called circulating liquid) and returning to the condensation section;
s2 (refining): oxidizing material: ethanol is prepared according to the following proportion of 1:1.2, putting the mixture into a refining kettle, and obtaining an azodiisobutyronitrile initiator through dissolution, crystallization, discharging, spin-drying and vacuum drying; recovering mother liquor, distilling to obtain ethanol, and recycling; and recovering distillation residual liquid (circulating liquid), and returning to the oxidation section for recycling.
The organic polymeric flocculant prepared by the experiment has the oil removal rate of 90.1 percent in wastewater.
Example 4
The preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: 15g of acrylic acid and 28g of tetramethylguanidine are heated, the temperature is raised, the mixture is stirred for 5 hours in a sealing and strong mechanical way, the tetramethylguanidine acrylate is obtained,
s2: fully dissolving 5g span80 in 100g cyclohexane solution, adding 30g acrylamide, 2g vinylguanamine and 12g synergist into a reactor, stirring and heating;
s3: adding 6g of initiator into the prepared S2 solution in the acrylic acid solution after the neutralization of the S1, and stirring to obtain an organic polymeric flocculant;
the heating temperature in S1 is 50 ℃.
And S2 is required to be continuously introduced with nitrogen for 2 hours.
The span80 is sorbitan monooleate.
The stirring rate was 600 revolutions per minute.
The reaction temperature of S2 is 60 ℃.
The reactor is made of stainless steel.
The preparation method of the synergist comprises the following steps:
15g of iron acrylate, 12g of sulfhydryl polyethylene glycol acrylate, 100g of cyclohexane solution, 7g of triethylamine are added into a reaction kettle, the temperature is raised, and nitrogen is continuously introduced for 3 hours, so as to obtain the synergist.
The reaction temperature was 70 ℃.
The preparation method of the initiator comprises the following steps:
s1 (condensation, oxidation): adding the oxidation circulating liquid, 6g of hydrazine hydrate and 15g of acetone cyanohydrin into a condensation kettle, stirring, and reacting at 50 ℃; after 2h, cl2 is introduced into the kettle through a Cl2 distributor, and after Cl2 3h, discharging is carried out; filtering, washing and spin-drying to obtain Cl2 material (i.e. crude azodiisobutyronitrile product); recovering waste liquid (called circulating liquid) and returning to the condensation section;
s2 (refining): oxidizing material: ethanol is prepared according to the following proportion of 1:1.2, putting the mixture into a refining kettle, and obtaining an azodiisobutyronitrile initiator through dissolution, crystallization, discharging, spin-drying and vacuum drying; recovering mother liquor, distilling to obtain ethanol, and recycling; and recovering distillation residual liquid (circulating liquid), and returning to the oxidation section for recycling.
The organic polymeric flocculant prepared by the experiment has the oil removal rate of 89.6% on the wastewater.
Comparative example 1
The procedure of example 3 was followed without the addition of span80 sorbitan monooleate;
the organic polymeric flocculant prepared by the experiment has the oil removal rate of 73.9% on the wastewater.
Comparative example 2
No synergist was added, otherwise the same as in example 3;
the organic polymeric flocculant prepared by the experiment has the oil removal rate of 63.7 percent in wastewater.
Comparative example 3
The same procedure as in example 3 is repeated, without the addition of initiator;
the organic polymeric flocculant prepared by the experiment has the oil removal rate of 77.5 percent in wastewater.
Claims (7)
1. The preparation process of organic polymer flocculant for water treatment includes the following steps:
s1: according to the weight portions, 10 to 15 portions of acrylic acid and 17 to 28 portions of tetramethylguanidine are heated, the temperature is raised, the mixture is sealed and strongly stirred mechanically for 3 to 5 hours to obtain the tetramethylguanidine acrylate,
s2: fully dissolving 1-5 parts of span80 in 50-100 parts of cyclohexane solution, adding 20-30 parts of acrylamide, 0.2-2 parts of vinylguanamine and 7-12 parts of synergist into a reactor, stirring and heating;
s3: adding 2-6 parts of initiator into the acrylic acid solution after S1 neutralization, and stirring to obtain an organic polymer flocculant;
the preparation method of the synergist comprises the following steps: according to the weight portions, 10-15 portions of iron acrylate, 5-12 portions of sulfhydryl polyethylene glycol acrylate, 50-100 portions of cyclohexane solution, 3-7 portions of triethylamine are added into a reaction kettle, and the temperature is raised and nitrogen is continuously introduced for 1-3 hours, thus obtaining the synergist.
2. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: the heating temperature in the step S1 is 40-50 ℃.
3. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: and the S2 is required to be continuously introduced with nitrogen for 0.5-2h.
4. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: the stirring speed is 500-600 rpm.
5. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: the reaction temperature of the S2 is 45-60 ℃.
6. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: the reactor is made of plastic, enamel, aluminum and stainless steel.
7. The method for preparing an organic polymeric flocculant for water treatment according to claim 1, wherein: the reaction temperature of the preparation method of the synergist is 60-70 ℃.
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| DD298764A5 (en) * | 1989-12-29 | 1992-03-12 | Institut Fuer Polymerenchemie "Erich Correns",De | PROCESS FOR FLAKING AND SEPARATION OF SUSPENSED SOLIDS AND / OR GELOESTER SUBSTANCES FROM HARD ACID GASES |
| JPH08143630A (en) * | 1994-11-17 | 1996-06-04 | Mitsui Toatsu Chem Inc | (meth)acrylamide polymer having aminotriazine ring on side chain |
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| CN113184845A (en) * | 2021-06-01 | 2021-07-30 | 浙江红狮环保股份有限公司 | Method for co-processing organic nitrogen-containing compound in cement kiln |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DD298764A5 (en) * | 1989-12-29 | 1992-03-12 | Institut Fuer Polymerenchemie "Erich Correns",De | PROCESS FOR FLAKING AND SEPARATION OF SUSPENSED SOLIDS AND / OR GELOESTER SUBSTANCES FROM HARD ACID GASES |
| JPH08143630A (en) * | 1994-11-17 | 1996-06-04 | Mitsui Toatsu Chem Inc | (meth)acrylamide polymer having aminotriazine ring on side chain |
| JP2004290969A (en) * | 2003-03-07 | 2004-10-21 | Sanyo Chem Ind Ltd | Polymer flocculant |
| CN1884315A (en) * | 2006-05-19 | 2006-12-27 | 浙江大学 | Anion type polymer containing tetramethylguanidine cation and its preparation method and uses |
| CA2954574A1 (en) * | 2017-01-13 | 2018-07-13 | Sortwell & Co. | Multi-acrylate anionic flocculants |
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