CN101899134B - Phosphate-free polyether scale inhibitor and preparation method thereof - Google Patents
Phosphate-free polyether scale inhibitor and preparation method thereof Download PDFInfo
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- CN101899134B CN101899134B CN 201010237731 CN201010237731A CN101899134B CN 101899134 B CN101899134 B CN 101899134B CN 201010237731 CN201010237731 CN 201010237731 CN 201010237731 A CN201010237731 A CN 201010237731A CN 101899134 B CN101899134 B CN 101899134B
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Abstract
The invention relates to a phosphate-free polyether scale inhibitor (APEX) which is a product of free radical polymerization of a polyether reaction monomer prepared by a lactone process and a monomer which contains a vinyl unsaturated double bond. The scale inhibitor comprises a structural general formula shown in the specification, wherein A is a constitutional repeating unit after the copolymerization of the monomer which contains the vinyl unsaturated double bond; R1 is H or a C1-C5 low-carbon alkyl; a value of P is 2 to 10; M is H<+>, K<+> or Na<+>; the polymerization degree x is 1 to 5,000; the polymerization degree y is 1 to 5,000; and the polymerization degree n is 1 to 100.
Description
Technical field
The present invention relates to prepare a kind of without phosphorus and biodegradable phosphate-free polyether scale inhibitor of stable performance, belong to the Scale inhibitors technology of preparing of water-treatment technology field, be applicable to the industrial colling recycle system.
Background technology
Along with the mankind to the pay attention to day by day of living environment and the increasingly stringent of environmental regulation, environmentally friendly water conditioner is subject to people's attention day by day, present a large amount of being widely used of phosphorous, nitrogenous Scale inhibitors, the amount reproduction of bacterium algae, the problem of environmental pollutions such as eutrophication of water body have been caused, therefore, the without phosphorus water conditioner of exploitation has become development trend.
Vinylformic acid-allyl polyether vitriol research of non-phosphorus scale inhibitor (AA-APES) has been invented by U.S. Betz company in 2002, this Scale inhibitors has the performance of resistance calcium phosphate scale.United States Patent (USP) 5062962 and United States Patent (USP) 5147555 show that poly-epoxy succinic acid is to CaCO
3, CaSO
4, BaSO
4Good scale inhibition effect is arranged, and have good corrosion mitigating effect, but very poor to the scale inhibition effect of calcium phosphate, when carrying out composite use with the organic phosphine corrosion inhibiting and descaling agent, increased the danger of calcium phosphate scale deposition.Contain amide group, carboxyl etc. in the Scale inhibitors that Chinese patent 200610056952.0 relates to, make it have good resistance CaSO
4The dirt performance also has the performance of certain dispersing iron oxide, has simultaneously well ageingly, but it is to resistance Ca
3(PO
4)
2The dirt performance is not good.Chinese patent CN101172720 discloses a kind of without phosphorus allyloxy polyether carboxylic acids antisludging agent and preparation method thereof, but can produce a large amount of reluctant inorganic abraum salts in this Scale inhibitors preparation process, easily cause secondary pollution and increase its industrial applications cost, the present invention adopts lactone one step esterification green reaction technique to make the polyether reactant monomer, and then has prepared a kind of excellent resistance Ca
3(PO
4)
2Without phosphorus and the biodegradable phosphate-free polyether scale inhibitor of dirt performance.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of phosphate-free polyether scale inhibitor and preparation method thereof, this Scale inhibitors is without phosphorus and biodegradable, and has excellent resistance Ca
3(PO
4)
2The dirt performance is a kind of eco-friendly phosphate-free polyether scale inhibitor.
Technical scheme: phosphate-free polyether scale inhibitor of the present invention (APEX) prepares the polyether reactant monomer with lactone process, carries out product after free-radical polymerized with this polyether reactant monomer and the monomer that contains the vinyl unsaturated double-bond, and its general structure is as follows:
Wherein: A is the repeated structural unit that contains behind the monomer copolymerization of vinyl unsaturated double-bond, R
1H or C
1～C
5Low-carbon alkyl, P value are that 2～10, M is H
+, K
+Or Na
+Polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and polymerization degree n is 1～100.
For example:
Following methods is adopted in the preparation of this phosphate-free polyether scale inhibitor (APEX):
Take allyl polyglycol monoether quality as benchmark, in the solid inorganic alkali adding reactor with allyl polyglycol monoether and 0.5～2 times of allyl polyglycol monoether quality, at N
2Under the atmosphere, behind 20～120 ℃ of alkalization 1～5h, add the lactone of 0.5～2 times of allyl polyglycol monoether quality, 30～150 ℃ of lower reaction 2～8h.Regulate the control temperature after 50 ℃～95 ℃, add the monomer that contains the vinyl unsaturated double-bond of 0.2～5 times of allyl polyglycol monoether quality, the distilled water of 0.1～5 times of allyl polyglycol monoether quality, the dropping mass percentage concentration is 5%～60% inorganic initiator solution behind the mixing, add-on without organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 0.5～5h drips off, drip off rear continuation at 50 ℃～95 ℃ lower reaction 0.5～5h, be chilled to room temperature, make phosphate-free polyether scale inhibitor, be called for short APEX, its solid content is 5～80wt%.
Lactone described in the preparation method of above-mentioned phosphate-free polyether scale inhibitor be beta-propiolactone, gamma-butyrolactone, γ-hexalactone, 6-caprolactone, γ-valerolactone, δ-valerolactone, δ-nonalactone, γ-nonyl lactone, γ-heptalactone, δ-hexanol lactone, in one or more combination.
The monomer that contains the vinyl unsaturated double-bond described in the preparation method of above-mentioned phosphate-free polyether scale inhibitor is one or more the combination in vinylformic acid, methacrylic acid, methyl acrylate, maleic anhydride, Propylene glycol monoacrylate, acrylamide, Methacrylamide, N methacrylamide, N-isopropoxy acrylamide, N,N-DMAA, toxilic acid, methylene-succinic acid, the N-pseudoallyl acrylamide.
Described in the preparation method of above-mentioned phosphate-free polyether scale inhibitor is one or more combination in Sodium Persulfate, ammonium persulphate, Potassium Persulphate, the hydrogen peroxide without organic initiators.
Mineral alkali described in the preparation method of above-mentioned phosphate-free polyether scale inhibitor is the combination of a kind of of NaOH, KOH or two kinds.
Beneficial effect: the phosphate-free polyether scale inhibitor that the present invention makes (APEX) has efficient restraining effect to the dirt of the phosphoric acid salt in cooling circulating water system layer.The compatibleness of phosphate-free polyether scale inhibitor is good, can with the composite uses of water conditioner such as organophosphate, zinc salt inhibiter, also can use separately.Static resistance Ca
3(PO
4)
2The dirt experiment is undertaken by China PetroChemical Corporation's " water coolant analysis and experimental technique " experiment 402, and the result is as follows:
High resistant Ca3 (PO4) 2 rates of Scale inhibitors kind
APEX 100.00％
AA-APES 99.73％
The result shows: phosphate-free polyether scale inhibitor (APEX) is suitable with the products A A-APES effect of the U.S. up-to-date resistance Ca3 (PO4) 2 dirts, but APEX is without phosphorus, long-term, high-dose uses the eutrophication that can not cause water body, and produce without abraum salt in the preparation process of APEX, technique is simple, production cost is low.
Embodiment
Phosphate-free polyether scale inhibitor of the present invention prepares the polyether reactant monomer with lactone process, and the product that carries out after free-radical polymerized with this polyether reactant monomer and the monomer that contains the vinyl unsaturated double-bond is phosphate-free polyether scale inhibitor (APEX), and its general structure is as follows:
Wherein: A is the repeated structural unit that contains behind the monomer copolymerization of vinyl unsaturated double-bond, R
1H or C
1～C
5Low-carbon alkyl, P value are that 2～10, M is H
+, K
+Or Na
+, polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and polymerization degree n is 1～100.
The preparation method of phosphate-free polyether scale inhibitor of the present invention is:
Take allyl polyglycol monoether quality as benchmark, in the solid inorganic alkali adding reactor with allyl polyglycol monoether and 0.5～2 times of allyl polyglycol monoether quality, at N
2Under the atmosphere, behind 20～120 ℃ of alkalization 1～5h, add the lactone of 0.5～2 times of allyl polyglycol monoether quality, 30～150 ℃ of lower reaction 2～8h; Regulate the control temperature after 50 ℃～95 ℃, the distilled water that contains vinyl unsaturated double-bond monomer, 0.1～5 times of allyl polyglycol monoether quality that adds 0.2～5 times of allyl polyglycol monoether quality, the dropping mass percentage concentration is 5%～60% inorganic initiator solution behind the mixing, add-on without organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 0.5～5h drips off, drip off rear continuation at 50 ℃～95 ℃ lower reaction 0.5～5h, be chilled to room temperature, make phosphate-free polyether scale inhibitor, its solid content is 5～80wt%.
Example 1: in the reactor of N2 protection, add 100g allyl polyglycol monoether, 80gNaOH; behind 50 ℃ of alkalization 2h; add the 120g gamma-butyrolactone in 80 ℃ of lower reaction 6h; add 150g distilled water; drip respectively simultaneously 80g maleic anhydride (being dissolved in 150g distilled water) and 6g Sodium Persulfate (being dissolved in 50g distilled water), after dropwising, continue at 80 ℃ of lower reaction 3h; after being down to room temperature, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 99.87%.
Example 2: in the reactor of N2 protection, add 150g allyl polyglycol monoether, 140g NaOH; behind 60 ℃ of alkalization 3h; add the 160g γ-nonyl lactone in 60 ℃ of lower reaction 8h; add 200g distilled water; drip respectively simultaneously 60g methacrylic acid (being dissolved in 100g distilled water) and 5g Potassium Persulphate (being dissolved in 50g distilled water), after dropwising temperature is increased to 90 ℃, continue reaction 5h; after being down to room temperature, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 99.24%.
Example 3: at N
2Add 140g allyl polyglycol monoether, 80gNaOH in the reactor of protection; behind 60 ℃ of alkalization 1h; add the 120g 6-caprolactone in 80 ℃ of reaction 6h; add 180g distilled water; drip respectively simultaneously 100g vinylformic acid (being dissolved in 100g distilled water) and 5g Sodium Persulfate (being dissolved in 40g distilled water), after dropwising temperature is increased to 95 ℃, continue reaction 5h; after being down to room temperature, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 98.54%.
Example 4: at N
2Add 120g allyl polyglycol monoether, 140gKOH in the reactor of protection; behind 50 ℃ of alkalization 3h; add the 100g beta-propiolactone in 80 ℃ of reaction 2h; add 150g distilled water; drip respectively simultaneously 100g vinylformic acid (being dissolved in 100g distilled water) and 5g Potassium Persulphate (being dissolved in 40g distilled water), after dropwising temperature is increased to 90 ℃, continue reaction 4h; after being down to room temperature, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 99.14%.
Example 5: at N
2Add 100g allyl polyglycol monoether, 100gKOH in the reactor of protection; behind 40 ℃ of alkalization 3h; add the 120g δ-valerolactone in 110 ℃ of reaction 4h; add 120g distilled water after being cooled to 95 ℃; drip respectively simultaneously 100g vinylformic acid (being dissolved in 100g distilled water) and 5g Sodium Persulfate (being dissolved in 40g distilled water); dropwise rear continuation at 95 ℃ of lower reaction 5h, be down to room temperature after, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 99.52%.
Example 6: at N
2Add 150g allyl polyglycol monoether, 180gKOH in the reactor of protection, behind 60 ℃ of alkalization 4h, add 200g δ-nonalactone, at N
2Protection is lower to 70 ℃ of reaction 4h; add 200g distilled water; drip respectively simultaneously 150g Propylene glycol monoacrylate (being dissolved in 150g distilled water) and 8g Sodium Persulfate (being dissolved in 50g distilled water); after dropwising temperature is increased to 90 ℃; continue reaction 5h; after being down to room temperature, make phosphate-free polyether scale inhibitor (APEX).
The resistance Ca of gained APEX Scale inhibitors
3(PO
4)
2Rate is 99.39%.
Claims (4)
1. the preparation method of a phosphate-free polyether scale inhibitor is characterized in that:
Take allyl polyglycol monoether quality as benchmark, in the solid inorganic alkali adding reactor with allyl polyglycol monoether and 0.5～2 times of allyl polyglycol monoether quality, at N
2Under the atmosphere, behind 20～120 ℃ of alkalization 1～5h, add the lactone of 0.5～2 times of allyl polyglycol monoether quality, 30～150 ℃ of lower reaction 2～8h; Regulate the control temperature after 50 ℃～95 ℃, the distilled water that contains vinyl unsaturated double-bond monomer, 0.1～5 times of allyl polyglycol monoether quality that adds 0.2～5 times of allyl polyglycol monoether quality, the dropping mass percentage concentration is 5%～60% inorganic initiator solution behind the mixing, add-on without organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 0.5～5h drips off, drip off rear continuation at 50 ℃～95 ℃ lower reaction 0.5～5h, be chilled to room temperature, make phosphate-free polyether scale inhibitor, its solid content is 5～80wt%;
The general structure of this phosphate-free polyether scale inhibitor is:
Wherein: A is the repeated structural unit that contains behind the vinyl unsaturated double-bond monomer copolymerization, R
1H or C
1～C
5Low-carbon alkyl, P value are that 2～10, M is H
+, K
+Or Na
+, polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and polymerization degree n is 1～100;
The described vinyl unsaturated double-bond monomer that contains is one or more combination in vinylformic acid, methacrylic acid, methyl acrylate, maleic anhydride, the Propylene glycol monoacrylate.
2. the preparation method of a kind of phosphate-free polyether scale inhibitor according to claim 1 is characterized in that employed lactone among this preparation method is one or more combination in beta-propiolactone, gamma-butyrolactone, γ-hexalactone, 6-caprolactone, γ-valerolactone, δ-valerolactone, δ-nonalactone, γ-nonyl lactone, γ-heptalactone, the δ-hexanol lactone.
3. the preparation method of a kind of phosphate-free polyether scale inhibitor according to claim 2 is characterized in that described in this preparation method being one or more combination in Sodium Persulfate, ammonium persulphate, Potassium Persulphate, the hydrogen peroxide without organic initiators.
4. the preparation method of a kind of phosphate-free polyether scale inhibitor according to claim 2 is characterized in that the mineral alkali described in this preparation method is the combination of a kind of of NaOH, KOH or two kinds.
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| CN102086063B (en) * | 2010-12-21 | 2013-05-01 | 东南大学 | Green environment-friendly polyether carboxylic acid ester corrosion inhibition and scale inhibitor and preparation method thereof |
| CN102516472B (en) * | 2011-11-25 | 2013-11-20 | 东南大学 | Environment-friendly polyether antisludging agent and preparation method thereof |
| CN102674567B (en) * | 2012-05-16 | 2013-11-20 | 东南大学 | Environment-friendly dendritic polyether dirt dispersion agent and preparation method thereof |
| CN102786150A (en) * | 2012-08-01 | 2012-11-21 | 东南大学 | Fluorescent tracing phosphorus-free environment-friendly polyether multifunctional water treatment agent and preparation method thereof |
| CN102786154A (en) * | 2012-08-01 | 2012-11-21 | 东南大学 | Phosphorus-free polyether multifunctional water treatment agent and preparation method thereof |
| CN102786152A (en) * | 2012-08-01 | 2012-11-21 | 东南大学 | Fluorescently labeled phosphorus-free environment-friendly polyether water treatment agent and preparation method thereof |
| CN102786155A (en) * | 2012-08-01 | 2012-11-21 | 东南大学 | Environment-friendly polyethyleneglycol multifunctional water treatment agent and preparation method thereof |
| CN102786153A (en) * | 2012-08-01 | 2012-11-21 | 东南大学 | Phosphorus-free environment-friendly polyether multifunctional water treatment agent and preparation method thereof |
| CN102786151B (en) * | 2012-08-01 | 2013-11-27 | 东南大学 | Environment-friendly polyglycol ether multifunctional water treatment agent and preparation method thereof |
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