CN102504080A - Dispersing agent for reusing reclaimed water prepared from production wastewater as circulating cooling water and preparation method - Google Patents
Dispersing agent for reusing reclaimed water prepared from production wastewater as circulating cooling water and preparation method Download PDFInfo
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Abstract
The invention discloses a dispersing agent for reusing reclaimed water prepared from production wastewater as circulating cooling water and a preparation method of the dispersing agent through a copolymerization method. The dispersing agent is a mixture with multiple active groups and produced by multi-component copolymerization reaction; calcium carbonate and calcium phosphate crystals and organic microparticles can be effectively prevented from forming deposited scale through the adsorption and chelation effects between the dispersing agent and inorganic scaling microcrystals in water, such as calcium carbonate and calcium phosphate as well as the organic microparticles; the dispersing agent specifically meets the characteristics that the reclaimed water obtained after wastewater treatment is high in hardness and high in base and contains multiple complex organic matters, and effectively takes good scale inhibition and dispersion effects on a circulating water system for reclaimed water recycling, thereby obtaining good and long-acting treatment effect.
Description
Technical field
The invention belongs to polymer high efficiency dispersion agent technical field, especially relate to dispersion agent and preparation method that water in a kind of factory effluent system is back to recirculated cooling water.
Background technology
Middle water reuse has huge environment and economic benefit, is the modern technique of pure environmental protection, but enterprise's waste discharge is complicated different with treatment process because of originating; Cause processing back water quality to have nothing in common with each other, water quality is abominable, the characteristics that middle water self is had after the production wastewater treatment; Can bring very ill effect to circulating water system; Careless slightly, will have a strong impact on the circulating water treatment effect, and then have a strong impact on the operation of production system; Cause to stop production or equipment damage the scope of application and the usage quantity of water reuse in the serious restriction.
A lot of enterprises can adopt dispersion agent to come the micro substance that contains in the Control Circulation water system; But because of trade effluent in processing in the water process; Water quality is unstable; Foreign ion is numerous, and the existing dispersion agent in the industry is the micro substance in the Control Circulation water system effectively, the serious fouling and the corrosion that cause like phosphate radical, calcium ions and magnesium ions, basicity, cl ions and various flora and algae etc.
Summary of the invention
The technical problem that the present invention will solve provides that water is back to dispersion agent of recirculated cooling water and preparation method thereof in a kind of factory effluent system.
Water is back to the dispersion agent of recirculated cooling water in a kind of factory effluent system, and its general structure is following:
Wherein: m representes that 1～150 natural number, n represent that 1～50 natural number, p represent that 1～100 natural number, x represent 1～100 natural number, and the molecular weight of above-claimed cpd is 1000～20000.
Water is back to the preparation method of the dispersion agent of recirculated cooling water in the above-mentioned factory effluent system, may further comprise the steps, and wherein the dosage of each raw material all refers to parts by weight:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 30～36 parts of de-ionized water of productive use and 5～7.5 parts of Virahols are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add 8～12 parts of MALEIC ANHYDRIDEs then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 3～4 parts of methyl acrylates and 6～9 parts of vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 3～8 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 3～7 parts of AMPS and 15～18 parts of de-ionized water of productive use are put into the weighing bucket, be stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, No. 2 monomer solutions are sucked in No. 2 header tanks with vacuum pump; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 2.5～3.0 parts of initiators and 15～18 parts of de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; Bottoming liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams 12～15 parts of isopropanol water solutions;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 12～15 parts of de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
Preferably, said initiator is a kind of in ammonium persulphate, the Potassium Persulphate.
Preferably, water is back to the preparation method of the dispersion agent of recirculated cooling water in the above-mentioned factory effluent system, may further comprise the steps, and wherein the dosage of each raw material all refers to parts by weight:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 30～32 parts of de-ionized water of productive use and 6～7.5 parts of Virahols are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add 10～12 parts of MALEIC ANHYDRIDEs then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 3～3.5 parts of methyl acrylates and 6～7.5 parts of vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 3～8 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 3～5 parts of AMPS and 15～16 parts of de-ionized water of productive use are put into the weighing bucket, be stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, No. 2 monomer solutions are sucked in No. 2 header tanks with vacuum pump; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 2.5～2.8 parts of initiators and 15～16 parts of de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; Bottoming liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams 12～14 parts of isopropanol water solutions;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 12～14 parts of de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
Advantage of the present invention and effect: this dispersion agent is that the multi-component copolymer reaction generates the compounding substances with various active group; Through with water in absorption, the sequestering action of inorganic scaling microcrystal such as lime carbonate, calcium phosphate and organic microparticle; Can effectively stop lime carbonate, calcium phosphate crystal and organic particle to form the deposition dirt; It is high hard, high-alkali and contain the organic characteristics of numerous complicated that special accord with wastewater handles in the back there to be glassware for drinking water; Effectively the circulating water system of centering water reuse plays good scale inhibition, dissemination, obtains good, long lasting treatment effect; And this dispersion agent can with inhibition, scale inhibition agent good combination such as other organic carboxyl acid classes; Solve middle water and be back to use incidental fouling, etching problem in the recirculated water process; Water can be back to use circulating cooling system in the numerous complicated in order to make, and has realized the purpose of saving water and energy to greatest extent.
Embodiment
In order to understand the present invention, the present invention is described further below by concrete embodiment.
Water is back to the dispersion agent of recirculated cooling water in the factory effluent system of the present invention, and its general structure is:
Its preparation method is: an amount of vinylformic acid and AMPS, methyl acrylate, MALEIC ANHYDRIDE under about 70 ℃ to 100 ℃ environment, in the presence of initiator, are carried out copolymerization and make, and the reaction formula of copolyreaction is following:
Wherein, m representes that 1～150 natural number, n represent that 1～50 natural number, p represent that 1～100 natural number, x represent 1～100 natural number, and the molecular weight of above-claimed cpd is 1000～20000.
Embodiment one:
Water is back to the preparation method of the dispersion agent of recirculated cooling water in the factory effluent system, may further comprise the steps:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 300kg de-ionized water of productive use and 75kg Virahol are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add the 115kg MALEIC ANHYDRIDE then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 32kg methyl acrylate and 66kg vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 5 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 43kgAMPS and 150kg de-ionized water of productive use are put into the weighing bucket, are stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, with vacuum pump with in No. 2 header tanks of No. 2 monomer solution suctions; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 26kg ammonium persulphate and 150kg de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; Bottoming liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams the 120kg isopropanol water solution;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 120kg de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
Products obtained therefrom is that the massfraction of solid matter is 30% the aqueous solution, as analyzes the too high amount that can increase the de-ionized water of productive use of back product effective content, is adjusted into 30% back and uses.
Embodiment two:
Water is back to the preparation method of the dispersion agent of recirculated cooling water in the factory effluent system, may further comprise the steps:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 360kg de-ionized water of productive use and 75kg Virahol are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add the 120kg MALEIC ANHYDRIDE then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 40kg methyl acrylate and 90kg vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 6 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 70kgAMPS and 180kg de-ionized water of productive use are put into the weighing bucket, are stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, with vacuum pump with in No. 2 header tanks of No. 2 monomer solution suctions; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 30kg Potassium Persulphate and 180kg de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; End liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams the 150kg isopropanol water solution;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 150kg de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
Products obtained therefrom is that the massfraction of solid matter is 30% the aqueous solution, as analyzes the too high amount that can increase the de-ionized water of productive use of back product effective content, is adjusted into 30% back and uses.
Embodiment three:
Water is back to the preparation method of the dispersion agent of recirculated cooling water in the factory effluent system, may further comprise the steps:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 300kg de-ionized water of productive use and 50kg Virahol are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add the 80kg MALEIC ANHYDRIDE then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 30kg methyl acrylate and 60kg vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 3 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 30kgAMPS and 150kg de-ionized water of productive use are put into the weighing bucket, are stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, with vacuum pump with in No. 2 header tanks of No. 2 monomer solution suctions; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 25kg initiator and 150kg de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; End liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams the 130kg isopropanol water solution;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 130kg de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
Products obtained therefrom is that the massfraction of solid matter is 30% the aqueous solution, as analyzes the too high amount that can increase the de-ionized water of productive use of back product effective content, is adjusted into 30% back and uses.
Among all embodiment of the present invention, said initiator is a kind of in ammonium persulphate, the Potassium Persulphate.
The effect of dispersion agent of the present invention is verified through the dynamic anti-scale distributed test of following testing laboratory:
TP: with under the water quality; Add the medicament that contains different dispersion agents; Through dynamicanalog device in laboratory simulation actual cycle cooling system working condition operation, and dynamically monitor, the heat exchange tube wall heat transfer conditions in the simulation interchanger in the computing system, i.e. fouling resistance; Investigate the scale inhibition dispersion effect of dispersion agent
Test water is a water in certain enterprise's typical production, and water water quality is following in the test:
| Numbering | Project | Unit | Numerical value |
| 1 | pH | 7.5 | |
| 2 | Calcium ion | Mg/L is (with CaCO 3Meter) | 100 |
| 3 | Mg ion | Mg/L is (with CaCO 3Meter) | 120 |
| 4 | Total hardness | Mg/L is (with CaCO 3Meter) | 320 |
| 5 | Total alkalinity | Mg/L is (with CaCO 3Meter) | 200 |
| 6 | COD | mg/L | 40 |
| 7 | Phosphate radical | mg/L | 5 |
Test medicine adopts to add equivalent organic phosphoric acid and the different types of dispersion agent 30mg/L of equivalent, and control concentrates 3 times, moves after 72 hours, calculates fouling resistance, and carries out dynamic scale inhibition simultaneous test, and test-results is following:
National standard, fouling resistance is less than 3.44 * 10
-4m
2K/W
Can find out by above test; Novel dispersant is compared with existing common binary, terpolymer, after water is back to use circulating water system among the typical case, greatly reduces fouling resistance; Improved heat exchange efficiency, better scale inhibition dispersion effect has been arranged than present common binary, terpolymer.
The present invention is not limited to above-mentioned preferred forms, and other any identical with the present invention or akin products that anyone draws under enlightenment of the present invention all drop within protection scope of the present invention.
Claims (4)
1. water is back to the dispersion agent of recirculated cooling water in the factory effluent system, and it is characterized in that: this dispersion agent has the described general structure suc as formula (I):
Formula (I): m representes that 1～150 natural number, n represent that 1～50 natural number, p represent that 1～100 natural number, x represent 1～100 natural number, and the molecular weight of above-claimed cpd is 1000～20000.
According to claim 1 in the factory effluent system water be back to the preparation method of the dispersion agent of recirculated cooling water, it is characterized in that: may further comprise the steps, wherein the dosage of each raw material all refers to parts by weight:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 30～36 parts of de-ionized water of productive use and 5～7.5 parts of Virahols are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add 8～12 parts of MALEIC ANHYDRIDEs then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 3～4 parts of methyl acrylates and 6～9 parts of vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 3～8 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 3～7 parts of AMPS and 15～18 parts of de-ionized water of productive use are put into the weighing bucket, be stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, No. 2 monomer solutions are sucked in No. 2 header tanks with vacuum pump; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 2.5～3.0 parts of initiators and 15～18 parts of de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; Bottoming liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams 12～15 parts of isopropanol water solutions;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 12～15 parts of de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
3. be back to the preparation method of the dispersion agent of recirculated cooling water like water in the said factory effluent system of claim 2, it is characterized in that: said initiator is a kind of in ammonium persulphate, the Potassium Persulphate.
4. be back to the preparation method of the dispersion agent of recirculated cooling water like water in the said factory effluent system of claim 2, it is characterized in that: may further comprise the steps, wherein the dosage of each raw material all refers to parts by weight:
1) preparation of raw material with add
A. the liquid that feels secure is prepared and is added: at first 30～32 parts of de-ionized water of productive use and 6～7.5 parts of Virahols are sucked in the reaction kettle through vacuum pump successively; The interior liquid level of reaction kettle is positioned at more than the minimum level of stirring; Add 10～12 parts of MALEIC ANHYDRIDEs then from the reaction kettle ingress; Open and stir, be stirred to solid material under the normal temperature and fully dissolve;
B.1 number monomer solution preparation: 3～3.5 parts of methyl acrylates and 6～7.5 parts of vinylformic acid are sucked respectively in No. 1 header tank through vacuum pump, suck two kinds of raw materials after, vacuumized again 3～8 minutes, make two kinds of raw materials mix even, form No. 1 monomer solution;
C.2 number monomer solution preparation: 3～5 parts of AMPS and 15～16 parts of de-ionized water of productive use are put into the weighing bucket, be stirred to the solid dissolving and mix the back and form No. 2 monomer solutions, No. 2 monomer solutions are sucked in No. 2 header tanks with vacuum pump; Wherein AMPS refers to 2-acrylic amide-2-methyl propane sulfonic acid;
D. the preparation of initiator solution: 2.5～2.8 parts of initiators and 15～16 parts of de-ionized water of productive use are joined in the weighing bucket, after being stirred to solid dissolving and mixing, form initiator solution, initiator solution is drawn in No. 3 header tanks with vacuum pump;
2) copolyreaction
A. open the whisking appliance of reaction kettle, close by-pass valve under the condensing surface, feed 1～2kg/cm in the reacting kettle jacketing
2Steam; Bottoming liquid in the reaction kettle is heated to 70 ℃, opens the bottom valve of No. 3 header tanks, be added drop-wise to the initiator solution of 1/2nd in No. 3 header tanks in the reaction kettle fast; Monitoring temperature of charge when dripping; The rate of addition that keeps initiator solution and bottoming liquid temp steadily, add the initiator solution of 1/2nd in No. 3 header tanks after, close the bottom valve of No. 3 header tanks;
B. reactor temperature is raised to 80～85 ℃; Stop heating then, vapour condensation water in the chuck is all emitted, open the bottom valve of No. 1 header tank, No. 2 header tanks and No. 3 header tanks synchronously; With No. 1 monomer solution, No. 2 monomer solutions with remain 1/2nd initiator solution and splash in the reaction kettle; Keep rate of addition stable, the dropping time of No. 1 monomer solution and No. 2 monomer solutions was controlled in 3 hours, and the initiator solution of residue 1/2nd is later than No. 1 monomer solution and No. 2 monomer solutions were accomplished in 5 minutes; And in whole dropping process, the temperature in the reaction kettle is lower than 95 ℃;
C.1 after number monomer solution, No. 2 monomer solutions and initiator solution all are added dropwise to complete, open by-pass valve under the condensing surface, strengthen chuck inner vapor flow, making reactor temperature is 90～100 ℃, steams 12～14 parts of isopropanol water solutions;
After the distillation of d.c step finishes, feed water coolant in the chuck of reaction kettle, the temperature in the reaction kettle is dropped to below 60 ℃, add 12～14 parts of de-ionized water of productive use, stop to stir and cooling, at this moment, copolyreaction is accomplished in the reaction kettle, generates feed liquid;
E. the feed liquid that copolyreaction generates in the reaction kettle is carried out weighing and packing after stainless steel filtering net, the two-layer filtration of absorbent cotton.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103554361A (en) * | 2013-10-25 | 2014-02-05 | 中国海洋石油总公司 | Preparation method of high-efficiency calcium phosphate scale inhibitor |
| CN106574021A (en) * | 2014-09-22 | 2017-04-19 | 东亚合成株式会社 | Acrylic acid-based copolymer, method for producing same and water treatment agent |
| CN113980175A (en) * | 2021-12-27 | 2022-01-28 | 潍坊金石环保科技有限公司 | Preparation method of modified hydrolyzed polymaleic anhydride |
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| CN101921359A (en) * | 2010-09-29 | 2010-12-22 | 湖南省原子能农业应用研究所 | Polyacrylic acid or copolymer thereof and preparation method of polyacrylate or copolymer salt thereof |
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| CN101921359A (en) * | 2010-09-29 | 2010-12-22 | 湖南省原子能农业应用研究所 | Polyacrylic acid or copolymer thereof and preparation method of polyacrylate or copolymer salt thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554361A (en) * | 2013-10-25 | 2014-02-05 | 中国海洋石油总公司 | Preparation method of high-efficiency calcium phosphate scale inhibitor |
| CN103554361B (en) * | 2013-10-25 | 2016-03-30 | 中国海洋石油总公司 | A kind of preparation method of high-efficiency calcium phosphate scale inhibitor |
| CN106574021A (en) * | 2014-09-22 | 2017-04-19 | 东亚合成株式会社 | Acrylic acid-based copolymer, method for producing same and water treatment agent |
| CN106574021B (en) * | 2014-09-22 | 2019-05-14 | 东亚合成株式会社 | Acrylic acid series copolymer and its manufacturing method and water treatment agent |
| CN113980175A (en) * | 2021-12-27 | 2022-01-28 | 潍坊金石环保科技有限公司 | Preparation method of modified hydrolyzed polymaleic anhydride |
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