CN108640299A - A kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent - Google Patents
A kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent Download PDFInfo
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- CN108640299A CN108640299A CN201810405368.4A CN201810405368A CN108640299A CN 108640299 A CN108640299 A CN 108640299A CN 201810405368 A CN201810405368 A CN 201810405368A CN 108640299 A CN108640299 A CN 108640299A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation methods of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent, with N N-tert-butyl acrylamides, acrylic acid, 2 acrylamide, 2 methyl propane sulfonic acid etc. for raw material, terpolymer antisludging agent is prepared by free yl solution polymerizating method, it is raw materials used to press following weight：10 ~ 90 parts by weight of N N-tert-butyl acrylamides, 5 ~ 45 parts by weight of acrylic acid, 2 acrylamide, 2 methyl propane sulfonic acid, 5 ~ 45 parts by weight.Antisludging agent scale-inhibiting properties prepared by the present invention are good, can effectively prevent the inorganic salts such as silicate during oil exploitation, industrial water circulation and deposit scale problems in equipment surface.
Description
Technical field
The present invention relates to a kind of preparation methods of heavy duty detergent copolymer silicon dirt antisludging agent, belong to industrial water conditioning agent designing technique
Field.
Background technology
Often have the substances such as carbonate, heavy carbonate, sulfate and silicate in recirculated water, due to water it is continuous cycle and it is dense
Contracting, it is various also constantly to increase at the particle concentration of dirt, after reaching saturation solubility, will fouling, fouling can cause to recycle
The cooling effect of water declines, and deposit buildup can cause a series of harm such as equipment corrosion, seriously affect the normal of industrial equipment
Operation.Calcium carbonate, magnesium in recirculated water, the quality such as calcium sulfate, magne-scale are relatively fluffy, easily remove, but silicate scale
Compact structure can be more difficult to remove after being attached on equipment and duct wall, thus comparatively the presence of silicon dirt to circulation
Harm bigger.Reach ideal scale inhibition effect, it is also just particularly significant to choose suitable water treatment agent and application method.In order to
The generation for reducing silicon dirt in recirculated water, it is relatively inexpensive feasible method to add antisludging agent into circulation.
Antisludging agent mainly has phosphorus system and polycarboxylic acids two major classes.Organic phosphine scale inhibitor has scale inhibition effect to a variety of dirts, but wherein
P elements can lead to body eutrophication, to limit its application and development；Polycarboxylic acid antisludging agent mainly for calcium scale,
Scale-inhibiting properties are single, such as acrylic acid (AA)-maleic anhydride (MA) copolymer.The present invention is with N tert butyl acrylamide, and third
Olefin(e) acid, 2- acrylamide-2-methyl propane sulfonics etc. are raw material, and a kind of novel tertiary has been synthesized by aqueous free radical polymerization
Copolymer can effectively inhibit the inorganic salts such as silicate during oil exploitation, industrial water circulation to deposit fouling in equipment surface
Problem.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent, should
Antisludging agent scale-inhibiting properties are good, have good inhibiting effect to depositions such as silicates in solution, effectively maintain the normal of industrial equipment
Operation.
A kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent, it is characterised in that this method include with
Lower step:
1）5 parts ~ 45 parts acrylic acid, 5 parts ~ 45 parts 2- acrylamide-2-methylpro panesulfonic acids are dissolved in 200 parts by weight of deionized water
After be uniformly mixed, it is 7 ~ 8 that alkaline reagent, which is added, and adjusts its pH, adds 10 parts ~ 90 parts N tert butyl acrylamides, stirring is equal
It is even, 0.2 part of disodium ethylene diamine tetraacetate is added into mixed monomer solution, mixed solution is transferred to reaction after being completely dissolved
In kettle；
2）0.3 parts by weight of activated dose of urea nitrate is taken, is dissolved in wiring solution-forming in 10 parts by weight of deionized water respectively, it is spare；It stirs on side
While modified activated carbon fiber material is added to reaction kettle, it is then charged with nitrogen, solution is heated to 70 DEG C, activating agent is slow
Slowly it is alternately added in reaction kettle, is added dropwise in 80min, 85 DEG C of heating and isothermal reaction 2h stop reaction and be cooled to room temperature
Copolymer solution.Constant-temperature vacuum dries 12h at 50 DEG C after the multiple precipitating of solution methanol, decompression are filtered, and obtains product height
Acting type copolymer silicon dirt antisludging agent.
Advantageous effect：The present invention is with N tert butyl acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics etc.
A kind of preparation method of heavy duty detergent copolymer silicon dirt antisludging agent of Material synthesis, due to containing carboxylic in the polymer antisludging agent of synthesis
Base can form hydrogen bond with silicic acid molecule, make silicic acid molecule that can not be further formed larger silicic acid micelle；Amido can be with titanium dioxide
Si-OH of silicon face forms the chemical bonds such as hydrogen bond, influences the generation of silica；Sulfonic group can dissociate sulfonate radical in water
Anion, anion can be combined with metal cations such as calcium and magnesiums, and the silica in disperse water prevents fouling.In addition, be added
Modified activated carbon fiber material specific surface area acts synergistically with activating agent urea nitrate greatly, and deoxidizing capacity in situ is higher, Regenerated energy
Power is strong, introduces a large amount of acid oxygen-containing functional group after modified, has preferable characterization of adsorption, can more assemble in water
Incrustation ion.
Specific implementation mode
Embodiment 1
1）It is mixed after 40 parts of acrylic acid, 40 parts of 2- acrylamide-2-methylpro panesulfonic acids are dissolved in 200 parts by weight of deionized water
Even, it is 7 ~ 8 that alkaline reagent, which is added, and adjusts its pH, adds 20 parts of N tert butyl acrylamides, stirs evenly, to mixed list
0.2 part of disodium ethylene diamine tetraacetate is added in liquid solution, mixed solution is transferred in reaction kettle after being completely dissolved；
2）0.3 parts by weight of activated dose of urea nitrate is taken, is dissolved in wiring solution-forming in 10 parts by weight of deionized water respectively, it is spare；It stirs on side
While modified activated carbon fiber material is added to reaction kettle, it is then charged with nitrogen, solution is heated to 70 DEG C, activating agent is slow
Slowly it is alternately added in reaction kettle, is added dropwise in 80min, 85 DEG C of heating and isothermal reaction 2h stop reaction and be cooled to room temperature
Copolymer solution.Constant-temperature vacuum dries 12h at 50 DEG C after the multiple precipitating of solution methanol, decompression are filtered, and obtains product three
Membered copolymer silicon dirt antisludging agent.
Above-mentioned modified activated carbon fiber material preparation method is as follows：
It takes 0.5 parts by weight polyimides felt in beaker, the ammonium phosphate solution that 400 parts by weight mass fractions are 0.5% is added and impregnates
1h, taking-up drain, and are then loaded into the stainless steel reaction pipe of 68mm, 500 ~ 700 DEG C, permanent under 0.5kPa in nitrogen atmosphere
Warm 3h postcoolings obtain activated carbon fiber.By activated carbon fiber distilled water flushing 5 ~ 6 times, it is put into beaker distilled water and impregnates 6h
After filter moisture, taking-up, which is placed again into the beaker equipped with distilled water, boils 6h, changes a water every 0.5h, filters moisture, put
Enter baking oven, 60 DEG C of bakings are spare for 24 hours.Above-mentioned activated carbon fiber is put into microwave reactor, 40 parts by weight mixed acid solutions are added（Nitre
Acid is 1 with sulfuric acid volume ratio:3）, it is 400W in microwave power, temperature is microwave reaction 5min at 75 DEG C, will be lived after reaction
Property the cooling of carbon fiber room temperature, washed to supernatant and be in neutrality with distilled water, drained and be placed in 60 DEG C of baking oven dry 48h, i.e.,
Obtain modified active carbon fiber.
Embodiment 2
Identical with embodiment 1, difference is：45 parts of acrylic acid of addition, 45 parts of 2- acrylamide-2-methylpro panesulfonic acids,
10 parts of N tert butyl acrylamides.
Embodiment 3
Identical with embodiment 1, difference is：35 parts of acrylic acid of addition, 35 parts of 2- acrylamide-2-methylpro panesulfonic acids,
30 parts of N tert butyl acrylamides.
Embodiment 4
Identical with embodiment 1, difference is：30 parts of acrylic acid of addition, 30 parts of 2- acrylamide-2-methylpro panesulfonic acids,
40 parts of N tert butyl acrylamides.
Embodiment 5
Identical with embodiment 1, difference is：25 parts of acrylic acid of addition, 25 parts of 2- acrylamide-2-methylpro panesulfonic acids,
50 parts of N tert butyl acrylamides.
Embodiment 6
Identical with embodiment 1, difference is：20 parts of acrylic acid of addition, 20 parts of 2- acrylamide-2-methylpro panesulfonic acids,
60 parts of N tert butyl acrylamides.
Embodiment 7
Identical with embodiment 1, difference is：15 parts of acrylic acid of addition, 15 parts of 2- acrylamide-2-methylpro panesulfonic acids,
70 parts of N tert butyl acrylamides.
Embodiment 8
Identical with embodiment 1, difference is：10 parts of acrylic acid of addition, 10 parts of 2- acrylamide-2-methylpro panesulfonic acids,
80 parts of N tert butyl acrylamides.
Embodiment 9
Identical with embodiment 1, difference is：5 parts of acrylic acid of addition, 5 parts of 2- acrylamide-2-methylpro panesulfonic acids,
90 parts of N tert butyl acrylamides.
Comparative example 1
Identical with embodiment 1, difference is：Only it is added without modified activated carbon fiber material.
Comparative example 2
Identical with embodiment 1, difference is：It is added without ammonium phosphate solution when only preparing modified activated carbon fiber material.
Comparative example 3
Identical with embodiment 1, difference is：It is not forged under nitrogen atmosphere when only preparing modified activated carbon fiber material
It burns.
Comparative example 4
Identical with embodiment 1, difference is：Microwave reactor is not used when only preparing modified activated carbon fiber material.
Comparative example 5
Identical with embodiment 1, difference is：Acrylic acid is substituted for cinnamic acid when only preparing silicon dirt antisludging agent.
Comparative example 6
Identical with embodiment 1, difference is：It is added without disodium ethylene diamine tetraacetate when only preparing silicon dirt antisludging agent.
Comparative example 7
Identical with embodiment 1, difference is：Reaction temperature is adjusted to 90 DEG C when only preparing silicon dirt antisludging agent.
Comparative example 8
Identical with embodiment 1, difference is：It is not passed through nitrogen when only preparing silicon dirt antisludging agent.
Comparative example 9
Identical with embodiment 1, difference is：It is added without activating agent urea nitrate.
The silicon dirt antisludging agent prepared as follows with comparative example 1 ~ 9 to the embodiment of the present invention 1 ~ 9 is tested for the property：
Scale inhibitor performance evaluation is tested
Preparation mass concentration is 500mg/L（With SiO2Meter）Na2SiO3Solution takes 250mL solution to be put into polyethylene bottle,
2.5mg antisludging agents are added, adjusts pH value of solution, covers bottle cap, be placed in 30 DEG C of thermostatic water baths, rear solution is primary with 0.22 μm for 24 hours
Property water system filter filtering, with solubility SiO in the analysis method filtrates tested of the high content silicon of Hash2Content, while doing blank
Experiment, and scale inhibition performance is calculated as follows.
Wherein η is scale inhibition performance, ρ1For SiO in original solution2Concentration, mg/L；ρ2For blank solution SiO2 Concentration, mg/L；
ρ3To add solution S iO after antisludging agent2Concentration, mg/L.
Scale inhibitor performance evaluation result
As seen from the above table, when 40 parts by weight of acrylic acid, 45 parts by weight 2- acrylamide-2-methylpro panesulfonic acids, 10 weight are added
The antisludging agent prepared when part N tert butyl acrylamide is 88.24% to Na2SiO3 solution scale inhibition performances, and scale-inhibiting properties are best, when changing
When becoming acrylic acid, 2- acrylamide-2-methylpro panesulfonic acids, N tert butyl acrylamide three's parts by weight, scale inhibition performance is different
The reduction of degree, the possible reason is when N tert butyl acrylamide weight ratio increases, N tert butyl acrylamide monomer is empty
Between steric effect make polymerisation degree reduction, in addition carboxyl and it is sulfonic reduction also make antisludging agent scale-inhibiting properties weaken, drop
Low scale inhibition performance.The addition of the explanation of comparative example 1 ~ 4 modified activated carbon fiber material and the selection of preparation condition are to scale inhibition
Agent scale-inhibiting properties are affected, and the selection of raw material and synthesis condition is to antisludging agent scale inhibition when comparative example 5 ~ 8 illustrates to prepare antisludging agent
Performance has prominent influence.Comparative example 1 and 9 shows that the addition of its activating agent urea nitrate cooperates with work with modified activated carbon fiber material
With apparent, deoxidizing capacity in situ is higher, and power of regeneration is strong, introduces a large amount of acid oxygen-containing functional group after modified, has preferable
Characterization of adsorption, can more assemble the incrustation ion in water, substantially increase scale inhibition performance.
Claims (7)
1. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent, it is characterised in that this method includes following
Step:
1）5 parts ~ 45 parts acrylic acid, 5 parts ~ 45 parts 2- acrylamide-2-methylpro panesulfonic acids are dissolved in 200 parts by weight deionizations
It is uniformly mixed after water, it is 7 ~ 8 that alkaline reagent, which is added, and adjusts its pH, adds 10 parts ~ 90 parts N tert butyl acrylamides, and stirring is equal
It is even, 0.2 part of disodium ethylene diamine tetraacetate is added into mixed monomer solution, mixed solution is transferred to reaction after being completely dissolved
In kettle；
2）0.3 parts by weight of activated dose is taken, is dissolved in wiring solution-forming in 10 parts by weight of deionized water respectively, it is spare；While stirring to anti-
It answers kettle that modified activated carbon fiber material is added, is then charged with nitrogen, solution is heated to 70 DEG C, activating agent is slowly replaced
It is added in reaction kettle, is added dropwise in 80min, 85 DEG C of heating and isothermal reaction 2h stop reaction and be cooled to room temperature copolymer
Solution, constant-temperature vacuum dries 12h at 50 DEG C after the multiple precipitating of solution methanol, decompression are filtered, and obtains product ternary polymerization
Object silicon dirt antisludging agent.
2. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent according to claim 1, feature
It is that above-mentioned steps neutral and alkali reagent is one or more in sodium bicarbonate, saleratus.
3. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent according to claim 1, feature
It is in above-mentioned steps that reaction kettle is ceramic electric heating reaction kettle.
4. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent according to claim 1, feature
It is in above-mentioned steps that activating agent is urea nitrate.
5. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent according to claim 1, feature
It is in above-mentioned steps that mixing speed is 300 ~ 400r/min.
6. a kind of preparation method of the preparation method of heavy duty detergent copolymer silicon dirt antisludging agent according to claim 1, feature
It is that the modified activated carbon fiber material preparation method is as follows：
It takes 0.5 parts by weight polyimides felt in beaker, the ammonium phosphate solution that 400 parts by weight mass fractions are 0.5% is added and impregnates
1h, taking-up drain, and are then loaded into the stainless steel reaction pipe of 68mm, 500 ~ 700 DEG C, permanent under 0.5kPa in nitrogen atmosphere
Warm 3h postcoolings obtain activated carbon fiber.
7. by activated carbon fiber distilled water flushing 5 ~ 6 times, it is put into after beaker impregnates 6h with distilled water and filters moisture, take out again
It is put into the beaker equipped with distilled water and boils 6h, change a water every 0.5h, filter moisture, be put into baking oven, 60 DEG C of bakings are standby for 24 hours
With；
Above-mentioned activated carbon fiber is put into microwave reactor, 40 parts by weight mixed acid solutions are added, is 400W, temperature in microwave power
Degree is microwave reaction 5min at 75 DEG C, after reaction cools down activated carbon fiber room temperature, is washed to supernatant with distilled water and is in
Neutrality is drained and is placed in 60 DEG C of baking oven dry 48h to get modified active carbon fiber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912773A (en) * | 2021-11-29 | 2022-01-11 | 新疆大学 | Amide polycarboxylic acid water treatment agent, preparation method and application thereof, composite silicon scale-resistant water treatment agent and use method thereof |
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| JP2002061089A (en) * | 2000-08-16 | 2002-02-28 | Hakuto Co Ltd | Method for controlling scale in process for producing deinked waste paper pulp |
| CN101798146A (en) * | 2010-03-24 | 2010-08-11 | 王显平 | Solid composite sterilizing scale inhibiting agent |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002061089A (en) * | 2000-08-16 | 2002-02-28 | Hakuto Co Ltd | Method for controlling scale in process for producing deinked waste paper pulp |
| CN101798146A (en) * | 2010-03-24 | 2010-08-11 | 王显平 | Solid composite sterilizing scale inhibiting agent |
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| 赵亮: "聚合物硅垢阻垢剂的合成与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912773A (en) * | 2021-11-29 | 2022-01-11 | 新疆大学 | Amide polycarboxylic acid water treatment agent, preparation method and application thereof, composite silicon scale-resistant water treatment agent and use method thereof |
| CN113912773B (en) * | 2021-11-29 | 2023-04-07 | 新疆大学 | Amide polycarboxylic acid water treatment agent, preparation method and application thereof, composite silicon scale-resistant water treatment agent and use method thereof |
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Application publication date: 20181012 |