CN103145925A - Polyether phosphate environment-friendly water treatment agent and preparation method thereof - Google Patents
Polyether phosphate environment-friendly water treatment agent and preparation method thereof Download PDFInfo
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- CN103145925A CN103145925A CN2013101008701A CN201310100870A CN103145925A CN 103145925 A CN103145925 A CN 103145925A CN 2013101008701 A CN2013101008701 A CN 2013101008701A CN 201310100870 A CN201310100870 A CN 201310100870A CN 103145925 A CN103145925 A CN 103145925A
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Abstract
The invention discloses a polyether phosphate environment-friendly water treatment agent and a preparation method thereof and particularly relates to a non-phosphorus biodegradable water treatment agent which is suitable for an industrial circulation cooling water system and used for water quality corrosion inhibition and scale inhibition treatment. The water treatment agent provided by the invention is prepared after a polyether phosphate reaction monomer and a vinyl-contained unsaturated double-bond monomer are subjected to free radical polymerization; the polymer has the general formula shown in the specification, wherein A is a repetitive structural unit obtained after the vinyl-contained unsaturated double-bond monomer is copolymerized, the polymerization degree x ranges from 1 to 5000, the polymerization degree y ranges from 1 to 5000, the number of the repetitive structural units ranges from 1 to 100, and n is equal to 0, 1, 3 and 4. The polyether phosphate water treatment agent is good in compatibility, can be compounded with water treatment agents such as organic phosphate and a zinc salt corrosion inhibitor and can also be used independently.
Description
Technical field
The present invention relates to a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM) and preparation method thereof, is a kind of water conditioner that is applicable to the non-phosphate biodegradable of industrial circulating cooling water system, is particularly useful for the high calcium cooling water quality.
Background technology
In process water, the consumption of water coolant accounts for more than 60% of whole process water.Therefore, the cycles of concentration of raising circulating water system, minimizing rate of water make-up just become the most effective approach of Industrial Water Saving.But along with water circuit uses, the raising of recirculated water concentration rate, most of ionic concn that make up water is introduced is doubled and redoubled, and also systematic temperature raises, and the solubleness of some unusual solubleness salt has been reduced.In addition due to the variation of pH value, the impact of the factors such as pressure of impurity, system in water, the alkaline earth metal cation that contains in 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 the insoluble inorganic salt Deng negatively charged ion, very easily cause corrosion and the fouling of system.At present in industry, method commonly used is that to add a small amount of Scale inhibitors, Scale inhibitors be to prevent that incrustation scale and dirt from producing or suppressing the Water Treatment medicament of its deposition growing.
Usually the water treatment agent of use is the carboxylic acid polyalcohol of chemosynthesis, hydroxyl carboxylic compound and organophosphate, and the composite phosphorus such as inorganic phosphate is product.This series products drops into and is difficult for degraded in water body environment, and phosphorus causes serious pollution to environment, simultaneously, the eutrophication that phosphorus forms at a certain temperature can make and grow a large amount of microorganisms and algae in water body, and water quality constantly worsens, cause equipment corrosion, shorten the equipment cycle of operation and work-ing life.Therefore from the angle of Sustainable development and protection of the environment, Green Water Treatment Reagents is undoubtedly the inexorable trend of following water treatment field development.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 invention 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 phosphorus-free green water conditioner poly-epoxy succinic acid (PESA) of abroad announcing at present in addition is to CaCO
3, CaSO
4, BaSO
4Scale inhibition effect is preferably arranged, and the characteristics such as biological degradability is good, applied range.But owing to being 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 danger of calcium phosphate scale deposition; And the corrosion inhibition of this type of Scale inhibitors is general.Therefore, exploitation is a kind of has an inhibition without phosphorus important topic that has become the research of domestic and international water treatment agent without nitrogen environmental type water conditioner of be widely used in industrial circulating water system of scale inhibition dual-use function of holding concurrently.
The present invention adopts double carboxy acid esterization method green reaction technique 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 water conditioner of good corrosion inhibition.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of polyether carboxylate class environment-friendly type water treatment agent and preparation method thereof, this water conditioner non-phosphate biodegradable has excellent resistance Ca
3(PO
4)
2, CaCO
3, CaSO
4The dirt effect has good corrosion inhibition simultaneously, and is environmentally friendly.
Technical scheme: polyether carboxylate class environment-friendly type water treatment agent of the present invention (APEM) is to carry out free-radical polymerized rear getting with polyether carboxylate reaction monomers and the monomer that contains the vinyl unsaturated double-bond, and this polymkeric substance general formula is:
Wherein: A is the repeated structural unit that contains after the monomer copolymerization of vinyl unsaturated double-bond, and polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and number of repeat unit m is that 1～100, n is 0,1,3,4.
The preparation method of above-mentioned polyether carboxylate class environment-friendly type water treatment agent is:
At N
2Under atmosphere, take allyl polyglycol monoether quality as benchmark, two carboxylic acids of allyl polyglycol monoether and 0.05～5 times of allyl polyglycol monoether quality are added in reactor, the esterifying catalyst that adds again 0.001～0.05 times of allyl polyglycol monoether quality, react 1～10h under 60～160 ℃, get the polyether carboxylate reaction monomers.After temperature of reaction is transferred to 50～95 ℃, add again 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, after mixing, the dropping mass percentage concentration is 5%～50% inorganic initiator solution, add-on without organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 1～5h drips off, drip off rear continuation and react 0.5～10h under 50～95 ℃, be chilled to room temperature, making solid content is a kind of polyether carboxylate class environment-friendly type water treatment agent of 5～70wt%.
The monomer that contains the vinyl unsaturated double-bond described in the preparation method of above-mentioned polyether carboxylate class environment-friendly type water treatment agent is one or more combination of vinylformic acid, methacrylic acid, methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, maleic anhydride, Propylene glycol monoacrylate, toxilic acid, methylene-succinic acid; Described esterifying catalyst is a kind of in sulfur oxychloride, DMF, p-methyl benzenesulfonic acid; Described without organic initiators be Sodium Persulfate, Potassium Persulphate, lay particular stress on-sulfinic acid sodium, lay particular stress on-sulfinic acid potassium, one or more combination in persulfonic acid sodium, persulfonic acid potassium, hydrogen peroxide.
Beneficial effect: water conditioner of the present invention (APEM) has following excellent properties:
(1) raw material of synthetic polymer is easy to get, and the not phosphorous eutrophy element of this polyether carboxylate class water conditioner, has good biodegradability, is a kind of novel Green Water Treatment Reagents.Its preparation technology's green environment is friendly, and 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, and the catalyzer of employing simply is easy to get.
(2) contain the strong polyether group of wetting ability in this polyether carboxylate class water conditioner structure, and can with the carboxylic acid ion of calcium ion chelating, the calcium phosphate in industrial circulating cooling water system, calcium carbonate and calcium sulfate scale are had efficient restraining effect.
(3) compatibleness of this polyether carboxylate class water conditioner 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 calcium 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 ".
Embodiment 1: at N
2Add 100g allyl polyglycol monoether in the reactor of protection; add 100g hexanodioic acid and 0.5g p-methyl benzenesulfonic acid to react 2.5h under 70 ℃; add 80g maleic anhydride (being dissolved in 100g water) and 100g water under 70 ℃; drip 12g Sodium Persulfate (being dissolved in 50g water) after mixing; after dropwising; continuation is reacted 3h under 80 ℃, after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
When the APEM of gained is 8mg/L at dosage, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.5%, to CaCO
3Scale inhibition performance is 93.8%, to CaSO
4Scale inhibition performance is 99.5%, is 88.5% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Embodiment 2: at N
2Add 100g allyl polyglycol monoether in the reactor of protection, add 120g oxalic acid and 0.6g sulfur oxychloride and 0.1gN; dinethylformamide reacts 3h under 60 ℃; add 50g vinylformic acid (being dissolved in 100g water) and 160g water under 60 ℃; drip 10g Potassium Persulphate (being dissolved in 40g water) after mixing; temperature is increased to 90 ℃ after dropwising; continue reaction 5h, after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
Gained APEM Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.9%, to CaCO
3Scale inhibition performance is 94.6%, to CaSO
4Scale inhibition performance is 98.7%., can reach 89.5% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Embodiment 3: at N
2Add 110g allyl polyglycol monoether in the reactor of protection, add 130g propanedioic acid and 1g p-methyl benzenesulfonic acid in 100 ℃ of reaction 2h; after being down to 70 ℃, temperature adds 110g butyl acrylate (being dissolved in 100g water) and 190g water; drip 10g Sodium Persulfate (being dissolved in 50g water) after mixing; temperature is increased to 95 ℃ after dropwising; continue reaction 2h; after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
Gained APEM 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 93.2%, to CaSO
4Scale inhibition performance is 98.7%, can reach 88.7% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Embodiment 4: at N
2Add 180g allyl polyglycol monoether in the reactor of protection; add 90g oxalic acid and 0.2g sulfur oxychloride and 0.5gN; dinethylformamide is in 120 ℃ of reaction 2h; add 140g Propylene glycol monoacrylate (being dissolved in 140g water) and 100g water after being cooled to 70 ℃; drip 10g Sodium Persulfate (being dissolved in 60g water) after mixing; dropwise rear continuation and react 2.5h under 85 ℃, after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
Gained APEM 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 95.4%, to CaSO
4Scale inhibition performance is 99.3%, can reach 89.5% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Embodiment 5: at N
2Add 150g allyl polyglycol monoether in the reactor of protection, add 60g pentanedioic acid and 0.3g sulfur oxychloride and 0.3gN, dinethylformamide is at N
2React 1.5h in 130 ℃ under protection; after being down to 60 ℃, temperature adds 100g methylene-succinic acid hydroxypropyl acrylate (being dissolved in 100g water) and 220g water; drip 12g Sodium Persulfate (being dissolved in 50g water) after mixing; temperature is increased to 90 ℃ after dropwising; continue reaction 5h; after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
Gained APEM Scale inhibitors is when dosage is 8mg/L, to Ca
3(PO
4)
2Scale inhibition performance can reach 99.7%, to CaCO
3Scale inhibition performance is 96.5%, to CaSO
4Scale inhibition performance is 99.7%, can reach 88.6% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Embodiment 6: at N
2Add 100g allyl polyglycol monoether in the reactor of protection; add 80g propanedioic acid and 0.8g p-methyl benzenesulfonic acid to react 3h under 70 ℃; add 140g toxilic acid (being dissolved in 130g water) and 100g water under 70 ℃; drip 8g Sodium Persulfate (being dissolved in 50g water) after mixing; after dropwising; temperature is increased under 90 ℃ reacts 5h, after being down to room temperature, make a kind of polyether carboxylate class environment-friendly type water treatment agent (APEM).
Gained APEM 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 91.6%, to CaSO
4Scale inhibition performance is 98.9%, can reach 86.5% to the corrosion inhibition rate of carbon steel (regulation that meets HG/T3523).
Claims (5)
1. a polyether carboxylate class environment-friendly type water treatment agent, is characterized in that this water conditioner is to carry out free-radical polymerized rear getting with polyether carboxylate reaction monomers and the monomer that contains the vinyl unsaturated double-bond, and this polymkeric substance general formula is as follows:
Wherein: A is the repeated structural unit that contains after the monomer copolymerization of vinyl unsaturated double-bond, and polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and number of repeat unit m is that 1～100, n is 0,1,3,4.
2. the preparation method of an a kind of polyether carboxylate class environment-friendly type water treatment agent as claimed in claim 1 is characterized in that this preparation method is:
At N
2Under atmosphere, take allyl polyglycol monoether quality as benchmark, two carboxylic acids of allyl polyglycol monoether and 0.05～5 times of allyl polyglycol monoether quality are added in reactor, the esterifying catalyst that adds again 0.001～0.05 times of allyl polyglycol monoether quality, react 1～10h under 60～160 ℃, get the polyether carboxylate reaction monomers; After temperature of reaction is transferred to 50～95 ℃, add again 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, after mixing, the dropping mass percentage concentration is 5%～50% inorganic initiator solution, add-on without organic initiators is 0.01～0.5 times of allyl polyglycol monoether quality, 1～5h drips off, drip off rear continuation and react 0.5～10h under 50～95 ℃, be chilled to room temperature, making solid content is the polyether carboxylate class environment-friendly type water treatment agent of 5～70wt%.
3. the preparation method of a kind of polyether carboxylate class environment-friendly type water treatment agent according to claim 2 is characterized in that the two carboxylic acids described in this preparation method are a kind of in oxalic acid, propanedioic acid, pentanedioic acid or hexanodioic acid.
4. the preparation method of a kind of polyether carboxylate class environment-friendly type water treatment agent according to claim 2, the combination of one or more that it is characterized in that the described monomer that contains the vinyl unsaturated double-bond is vinylformic acid, methacrylic acid, methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, maleic anhydride, Propylene glycol monoacrylate, toxilic acid or methylene-succinic acid.
5. the preparation method of a kind of polyether carboxylate class environment-friendly type water treatment agent according to claim 2 is characterized in that described esterifying catalyst is a kind of in sulfur oxychloride, DMF or p-methyl benzenesulfonic acid; Described without organic initiators be Sodium Persulfate, Potassium Persulphate, lay particular stress on-sulfinic acid sodium, lay particular stress on-sulfinic acid potassium, one or more combination in persulfonic acid sodium, persulfonic acid potassium or hydrogen peroxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944602A (en) * | 2015-06-05 | 2015-09-30 | 东南大学 | Environment-friendly polyether water treatment agent for sea water desalination film and preparation method for environment-friendly polyether water treatment agent |
| CN108586675A (en) * | 2018-05-19 | 2018-09-28 | 兰州交通大学 | A kind of preparation of novel environment friendly high-efficiency type water quality stabilizer RG-20 |
| CN112176349A (en) * | 2019-07-03 | 2021-01-05 | 中国石油化工股份有限公司 | Non-phosphorus corrosion inhibitor composition, non-phosphorus corrosion inhibitor and application thereof |
| CN114105322A (en) * | 2020-08-27 | 2022-03-01 | 中国石油天然气股份有限公司 | Scale inhibitor composition, scale inhibitor and preparation method thereof |
| CN114262896A (en) * | 2021-10-11 | 2022-04-01 | 安徽工业大学 | Non-ionic polymer carboxylate corrosion inhibitor and preparation method thereof |
| CN114292408A (en) * | 2021-12-07 | 2022-04-08 | 恩泰环保科技（常州）有限公司 | Hyperbranched phosphorus-free water treatment agent containing tertiary amine and preparation method and application thereof |
| CN116693072A (en) * | 2023-08-01 | 2023-09-05 | 杭州尚善若水环保科技有限公司 | Water treatment agent |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944602A (en) * | 2015-06-05 | 2015-09-30 | 东南大学 | Environment-friendly polyether water treatment agent for sea water desalination film and preparation method for environment-friendly polyether water treatment agent |
| CN108586675A (en) * | 2018-05-19 | 2018-09-28 | 兰州交通大学 | A kind of preparation of novel environment friendly high-efficiency type water quality stabilizer RG-20 |
| CN112176349A (en) * | 2019-07-03 | 2021-01-05 | 中国石油化工股份有限公司 | Non-phosphorus corrosion inhibitor composition, non-phosphorus corrosion inhibitor and application thereof |
| CN112176349B (en) * | 2019-07-03 | 2022-05-17 | 中国石油化工股份有限公司 | Non-phosphorus corrosion inhibitor composition, non-phosphorus corrosion inhibitor and application thereof |
| CN114105322A (en) * | 2020-08-27 | 2022-03-01 | 中国石油天然气股份有限公司 | Scale inhibitor composition, scale inhibitor and preparation method thereof |
| CN114105322B (en) * | 2020-08-27 | 2023-10-27 | 中国石油天然气股份有限公司 | Scale inhibitor composition, scale inhibitor and preparation method thereof |
| CN114262896A (en) * | 2021-10-11 | 2022-04-01 | 安徽工业大学 | Non-ionic polymer carboxylate corrosion inhibitor and preparation method thereof |
| CN114292408A (en) * | 2021-12-07 | 2022-04-08 | 恩泰环保科技（常州）有限公司 | Hyperbranched phosphorus-free water treatment agent containing tertiary amine and preparation method and application thereof |
| CN116693072A (en) * | 2023-08-01 | 2023-09-05 | 杭州尚善若水环保科技有限公司 | Water treatment agent |
| CN116693072B (en) * | 2023-08-01 | 2023-10-13 | 杭州尚善若水环保科技有限公司 | water treatment agent |
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Application publication date: 20130612 |