CN102086063A - Green environment-friendly polyether carboxylic acid ester corrosion inhibition and scale inhibitor and preparation method thereof - Google Patents
Green environment-friendly polyether carboxylic acid ester corrosion inhibition and scale inhibitor and preparation method thereof Download PDFInfo
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- CN102086063A CN102086063A CN 201010598209 CN201010598209A CN102086063A CN 102086063 A CN102086063 A CN 102086063A CN 201010598209 CN201010598209 CN 201010598209 CN 201010598209 A CN201010598209 A CN 201010598209A CN 102086063 A CN102086063 A CN 102086063A
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Abstract
The invention relates to a green environment-friendly polyether carboxylic acid ester corrosion inhibition and scale inhibitor (APEL) and preparation method thereof. The corrosion and scale inhibitor is a phosphorus-free, nitrogen-free and biodegradable water treatment agent, which is applicable to industrial recirculated cooling water and is used for water quality corrosion inhibition and scale inhibition treatment. The corrosion inhibition scale inhibitor of the present invention is obtained by free radical copolymerization of polyether carboxylic acid ester reactive monomers and vinyl unsaturated double bond monomers, which comprise the following structural general formula: wherein A is monomer copolymerized constitutional repeating unit containing vinyl unsaturated double bond; R is H or C1 to C5 low carbon alkyl; the degree of polymerization of x is 1 to 5000; the degree of polymerization of y is 1 to 5000; repeating unit amount of m is 1 to 100. The carboxylic acid ester corrosion inhibition and scale inhibitor has good compatibleness, can be used alone or in combination with other water treatment agents, like organic phosphate, zinc salt corrosion inhibitor.
Description
Technical field
The present invention relates to a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL) and preparation method thereof, be a kind of without phosphorus, the no nitrogen of industrial circulating cooling water system, biodegradable water conditioner of being applicable to, the inhibition and the scale inhibition that are used for water quality are handled, and belong to the corrosion inhibiting and descaling agent technology of preparing of water-treatment technology field.
Background technology
Recirculating cooling water system in the industrial production, in the use because the influence of the factors such as pressure of the variation of the rising of the variation of the evaporation of moisture, pH value, temperature, flow velocity, the impurity in the water, system, alkaline earth metal cation that contains in the water such as Ca
2+, Mg
2+, Ba
2+With a small amount of other positively charged ions such as Fe
2+, Fe
3+, Cu
2+, Al
3+, Zn
2+Deng, can with water in SO
4 2-, CO
3 2-, HCO
3 -, OH
-, PO
4 3-, SiO
3 2-Generate insoluble inorganic salt such as Ca Deng negatively charged ion
3(PO
4)
2, CaCO
3, CaSO
4, Mg (OH)
2Deng, become dirt (being commonly called as incrustation scale) with deposited on surface of heat exchanger at pipeline, thereby cause the heat exchanger heat transfer efficiency to reduce and cause underdeposit corrosion.So the agent of use high-efficiency corrosion-mitigation scale-inhibition suppresses dirty thing formation and prevents metallic corrosion, be one of gordian technique that keeps the good operation of cooling water recirculation system; It also is the effective means that the control incrustation scale formed and prevented metallic corrosion in process water and the wastewater treatment.
Mainly concentrating on organic multicomponent phosphoric acid class Scale inhibitors and polycarboxylic acid Scale inhibitors aspect the Scale inhibitors research both at home and abroad at present, inhibiter mainly concentrates on organophosphorus, organic amine and compound corrosion inhibitor.The organic phosphates Scale inhibitors has stable chemical performance, ability comparatively high temps and pH value, advantages such as tangible molten limit effect and synergistic effect is arranged, but phosphorus is the nutrition source of bacterium and algae, contain the eutrophication that Phosphorus Scale inhibitors easily causes the environment waters, promote the growth of bacterium algae to form red tide and cause pollution of waterhead.Vinylformic acid-allyl polyether vitriol non-phosphorus scale agent (AA-APES) has been invented by U.S. Betz company in 2002, though this Scale inhibitors has the performance of good resistance calcium phosphate scale, but the shortcoming of this class Scale inhibitors is still to contain nutritive elements such as N, S in its structure, and long-term heavy dose of use still can cause the eutrophication of water body.Particularly enter 21 century, great revolutionary change has taken place in the developing direction of World chemical and chemical industry subject, and its sign is exactly the proposition of " Green Chemistry " notion.Therefore, developing the developing direction that without phosphorus, no nitrogen, environmental type corrosion inhibiting and descaling agent that biodegradability is good have become the 21 century water conditioner, also is the difficult point and the focus of research at present.The polycarboxylic acid Scale inhibitors has that scale inhibition effect is good, Heat stability is good and environmentally safe, generally is subject to people's attention.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.United States Patent (USP) 5062962 and 5147555 shows that poly-epoxy succinic acid (PESA) is to CaCO
3, CaSO
4, BaSO
4Scale inhibition effect is preferably arranged, and have characteristics such as biological degradability is good, applied range.But owing to be mainly carboxyl functional group in the poly-epoxy succinic acid molecular structure, single functional group has limited it and has disperseed the ability of iron, and the poor effect of resistance calcium phosphate when carrying out composite use with the organic phosphine corrosion inhibiting and descaling agent, has increased the sedimentary danger of calcium phosphate scale; The corrosion inhibition of this type of Scale inhibitors is general in addition.Therefore, develop a kind of hold concurrently without phosphorus no nitrogen environmental type corrosion inhibiting and descaling agent with the industrial cycle water system of extensively to be suitable for of scale inhibition dual-use function of inhibition that has, have important scientific meaning and great application value for the update of corrosion inhibiting and descaling agent.The present invention adopts succinyl oxide open loop method green reaction technology to make the polyether carboxylate reaction monomers, and then has prepared a kind of resistance Ca of excellence
3(PO
4)
2, CaCO
3, CaSO
4Dirt and have the environmental type polyether carboxylate corrosion inhibiting and descaling agent of good corrosion inhibition.
Summary of the invention
Technical problem:The purpose of this invention is to provide a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent, without phosphorus, the no nitrogen of this Scale inhibitors, biodegradable has excellent resistance Ca
3(PO
4)
2, CaCO
3, CaSO
4The dirt effect has good corrosion inhibition simultaneously, is a kind of eco-friendly environmental type corrosion inhibiting and descaling agent.
Technical scheme:A kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL) is to carry out free-radical polymerized back and get with polyether carboxylate reaction monomers 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, and R is H or C
1~ C
5Low-carbon alkyl.Polymerization degree x is 1 ~ 5000, and polymerization degree y is 1 ~ 5000, and number of repeat unit m is 1 ~ 100.
The preparation method of above-mentioned a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent is:
At N
2Under the atmosphere, be benchmark with allyl polyglycol monoether quality, in the succinyl oxide adding reactor with allyl polyglycol monoether and 0.05～5 times of allyl polyglycol monoether quality, 50 ~ 150 ℃ are reacted 1 ~ 10h down, get the polyether carboxylate reaction monomers.After temperature of reaction transferred to 60 ~ 95 ℃, add the monomer that contains the vinyl unsaturated double-bond of 0.2 ~ 5 times of allyl polyglycol monoether quality, the water of 0.1 ~ 5 times of allyl polyglycol monoether quality again, the dropping mass percentage concentration is 5%～60% inorganic initiator solution behind the mixing, the add-on of no organic initiators is 0.01 ~ 0.5 times of allyl polyglycol monoether quality, 0.5～5h drips off, dripping off the back continues to react 0.5～10h down at 60 ~ 95 ℃, be chilled to room temperature, making solid content is the environmental type polyether carboxylate corrosion inhibiting and descaling agent of 5 ~ 80wt%.
Contain one or more the combination that vinyl unsaturated double-bond monomer is vinylformic acid, methacrylic acid, methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, maleic anhydride, Propylene glycol monoacrylate, toxilic acid, methylene-succinic acid described in the preparation method of above-mentioned environmental type polyether carboxylate corrosion inhibiting and descaling agent.No organic initiators described in this preparation method is Sodium Persulfate, Potassium Persulphate, lay particular stress on-sulfinic acid sodium, lay particular stress on-sulfinic acid potassium, one or more the combination in the persulfonic acid sodium, persulfonic acid potassium, hydrogen peroxide.
Beneficial effect:Corrosion inhibiting and descaling agent of the present invention (APEL) has following excellent properties:
(1) eutrophy element such as not phosphorous, nitrogen of this polyether carboxylate corrosion inhibiting and descaling agent has the favorable biological degradability energy, is a kind of novel green water conditioner.Its preparation technology's green environment close friend, building-up process adopts environmental protection, inexpensive water as reaction solvent, and reaction process adopts " treating different things alike " mode, need not to separate, and is simple to operation, production cost is lower.
(2) contain the strong polyether group of wetting ability in this polyether carboxylate corrosion inhibiting and descaling agent structure, and can with the carboxylic acid ion of calcium ion chelating, the calcium phosphate in the industrial circulating cooling water system, lime carbonate and calcium sulfate dirt are had restraining effect efficiently.
(3) compatibleness of this polyether carboxylate corrosion inhibiting and descaling agent is good, can with the composite uses of water conditioner such as organophosphate, zinc salt inhibiter, also can use separately.
Embodiment
Static resistance Ca of the present invention
3(PO
4)
2The dirt experiment is undertaken by China PetroChemical Corporation's " water coolant analysis and experimental technique " experiment 402; The calculating of the lime carbonate in the scale-inhibiting properties test experiments, calcium sulfate scale inhibition performance is carried out according to " the oil and gas industry standard-SY/T5673-1993 of the People's Republic of China (PRC) "; The test of corrosion inhibition is with reference to " State Standard of the People's Republic of China GB/T18175-2000, the mensuration of water conditioner corrosion inhibition-rotary hanging plate method ".
Example 1:At N
2Add 100g allyl polyglycol monoether in the reactor of protection; add the 100g succinyl oxide and react 2.5h down in 70 ℃; 70 ℃ add 80g maleic anhydride (being dissolved in 100g water) and 100g water down; drip 12g Sodium Persulfate (being dissolved in 50g water) behind the mixing; after dropwising; continuation is at 80 ℃ of following reaction 3h, reduce to room temperature after, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
When the APEL of gained is 8mg/L at dosage, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.7%, to CaCO
3Scale inhibition performance is 94.8%, to CaSO
4Scale inhibition performance is 99.8%, is 89.5% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T 3523).
Example 2:At N
2Add 100g allyl polyglycol monoether in the reactor of protection, add 120g succinyl oxide reaction 3h under 60 ℃; 60 ℃ add 60g vinylformic acid (being dissolved in 100g water) and 150g water down; drip 10g Potassium Persulphate (being dissolved in 50g water) behind the mixing; after dropwising temperature is increased to 90 ℃; continue reaction 5h; after reducing to room temperature, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
Gained APEL Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.5%, to CaCO
3Scale inhibition performance is 94.6%, to CaSO
4Scale inhibition performance is 99.7%., carbon steel (is met HG/T's 3523
Regulation) corrosion inhibition rate can reach 89.2%.
Example 3:At N
2Add 110g allyl polyglycol monoether in the reactor of protection, add the 130g succinyl oxide in 100 ℃ of reaction 2h; after reducing to 70 ℃, temperature adds 100g butyl acrylate (being dissolved in 100g water) and 180g water; drip 10g Sodium Persulfate (being dissolved in 60g water) behind the mixing; after dropwising temperature is increased to 95 ℃; continue reaction 2h; after reducing to room temperature, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
Gained APEL Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 96.3%, to CaCO
3Scale inhibition performance is 91.2%, to CaSO
4Scale inhibition performance is 98.7%, can reach 88.9% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T 3523).
Example 4:At N
2Add 180g allyl polyglycol monoether in the reactor of protection; add the 90g succinyl oxide in 120 ℃ of reaction 2h; add 150g Propylene glycol monoacrylate (being dissolved in 150g water) and 100g water after being cooled to 70 ℃; drip 10g Sodium Persulfate (being dissolved in 50g water) behind the mixing; dropwising the back continues to react 2.5h down at 85 ℃; after reducing to room temperature, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
Gained APEL Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 97.5%, to CaCO
3Scale inhibition performance is 95.4%, to CaSO
4Scale inhibition performance is 99.3%, can reach 89.1% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T 3523).
Example 5:At N
2Add 150g allyl polyglycol monoether in the reactor of protection, add the 60g succinyl oxide, at N
2Protection is down in 130 ℃ of reaction 1.5h; after reducing to 70 ℃, temperature adds 100g methylene-succinic acid hydroxypropyl acrylate (being dissolved in 100g water) and 200g water; drip 12g Sodium Persulfate (being dissolved in 50g water) behind the mixing; after dropwising temperature is increased to 90 ℃; continue reaction 5h; after reducing to room temperature, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
Gained APEL Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.6%, to CaCO
3Scale inhibition performance is 96.2%, to CaSO
4Scale inhibition performance is 99.7%, can reach 88.4% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T 3523).
Example 6:At N
2Add 100g allyl polyglycol monoether in the reactor of protection; add the 80g succinyl oxide and react 3h down in 70 ℃; 70 ℃ add 130g toxilic acid (being dissolved in 130g water) and 100g water down; drip 8g Sodium Persulfate (being dissolved in 50g water) behind the mixing; after dropwising; temperature is increased to 80 ℃ of down reaction 5h, reduce to room temperature after, make environmental type polyether carboxylate corrosion inhibiting and descaling agent (APEL).
Gained APEL Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 97.3%, to CaCO
3Scale inhibition performance is 91.6%, to CaSO
4Scale inhibition performance is 98.9%, can reach 86.9% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T 3523).
Claims (4)
1. environmental type polyether carboxylate corrosion inhibiting and descaling agent is characterized in that this corrosion inhibiting and descaling agent is to carry out free-radical polymerized back and get with polyether carboxylate reaction monomers 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, and R is H or C
1～C
5Low-carbon alkyl, polymerization degree x are 1～5000, and polymerization degree y is 1～5000, and number of repeat unit m is 1～100.
2. the preparation method of an a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent as claimed in claim 1 is characterized in that this preparation method is:
At N
2Under the atmosphere, be benchmark with allyl polyglycol monoether quality, in the succinyl oxide adding reactor with allyl polyglycol monoether and 0.05～5 times of allyl polyglycol monoether quality, 50～150 ℃ are reacted 1～10h down, get the polyether carboxylate reaction monomers; After temperature of reaction transferred to 60～95 ℃, add the monomer that contains the vinyl unsaturated double-bond of 0.2～5 times of allyl polyglycol monoether quality, the water of 0.1～5 times of allyl polyglycol monoether quality again, the dropping mass percentage concentration is 5%～60% inorganic initiator solution behind the mixing, the add-on of no organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 0.5～5h drips off, dripping off the back continues to react 0.5～10h down at 60～95 ℃, be chilled to room temperature, making solid content is the environmental type polyether carboxylate corrosion inhibiting and descaling agent of 5～80wt%.
3. the preparation method of a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent according to claim 2 is characterized in that one or more the combination that vinyl unsaturated double-bond monomer is vinylformic acid, methacrylic acid, methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, maleic anhydride, Propylene glycol monoacrylate, toxilic acid or methylene-succinic acid that contains described in this preparation method.
4. the preparation method of a kind of environmental type polyether carboxylate corrosion inhibiting and descaling agent according to claim 2, it is characterized in that the no organic initiators described in this preparation method be Sodium Persulfate, Potassium Persulphate, lay particular stress on-sulfinic acid sodium, lay particular stress on-sulfinic acid potassium, one or more the combination in persulfonic acid sodium, persulfonic acid potassium or the hydrogen peroxide.
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