CN101786733A - Propenol itaconic acid sulfonate multipolymer scale inhibiting agent and preparation method thereof - Google Patents
Propenol itaconic acid sulfonate multipolymer scale inhibiting agent and preparation method thereof Download PDFInfo
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- CN101786733A CN101786733A CN 201010141952 CN201010141952A CN101786733A CN 101786733 A CN101786733 A CN 101786733A CN 201010141952 CN201010141952 CN 201010141952 CN 201010141952 A CN201010141952 A CN 201010141952A CN 101786733 A CN101786733 A CN 101786733A
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- sulfonate
- propenol
- methylene
- itaconic acid
- succinic acid
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Abstract
The invention relates to a polynary scale and corrosion inhibiting agent and a preparation method thereof, in particular to a propenol itaconic acid sulfonate multipolymer scale inhibitin agent and a preparation method thereof. The scale inhibiting agent is characterized by being prepared from propenol, itaconic acid and sulfonate through aqueous polymerization under an initiating agent system, wherein by taking the mass of the itaconic acid as a reference, the addition of the sulfonate is 10-50 percent, the addition of the propenyl is 5-20 percent, the addition of the initiating agent is 5-30 percent, and the addition of sodium hypophosphite is 5-30 percent. In the invention, the itaconic acid is used as a raw material and is subjected to the aqueous polymerization with the propenyl and the sulfonate, and the invention has simple production process, fewer product residual monomers and no three waste exhausts. A polymer prepared by using the method has high-efficiency inhibiting effect on the formation and the adhesion of scale layers of carbonates, sulfates, phosphates, silicates, and the like in a cooling water system and good dispersant effect on iron oxide, sludge, and the like.
Description
Technical field
The present invention relates to a kind of polynary anti-incrustation corrosion inhibitor and method for making, specifically is a kind of propenol itaconic acid sulfonate multipolymer scale inhibiting agent and method for making thereof.
Background technology
In recent years, along with China's rapid economy development, the scarcity of water resources and pollution had become one of important factor that influences China's Economic development.More than 300 big and medium-sized cities lack of water arranged at present, wherein the city sent out such as 1/3 city serious water shortage, especially coastal cities, east.In a lot of local groundwater resource exhaustions, the foreign water resource-constrained, sewage is administered in water saving and the new water source of exploitation has meaning of equal importance.Water is industrial heat exchange system heat-eliminating medium commonly used, the industrial circulating cooling water consumption accounts for about 70% of industrial water consumption, improves the recirculated cooling water service efficiency, not only can significantly save water resources, reduce a large amount of heat energy of draining in vain simultaneously, favourable promoting economic development with recirculated water.
(for example: Ca not only contain alkaline earth metal cation in the recirculated water
2+, Mg
2+, Ba
2+) and a small amount of other positively charged ion (Fe for example
2+, Fe
3+, Cu
2+, Zn
2+Deng), SO is also arranged simultaneously
4 2-, CO
3 2-, OH-, HCO
3-, PO
43-, SiO
3 2-Deng becoming dirty negatively charged ion.In circulating water system, because the evaporation of moisture, medium pH, temperature variation, influences such as flow velocity variation, some insoluble inorganic salt incrustation scale such as CaCO
3, MgCO
3, CaSO
4, Ca
3(PO
4)
2, Mg (OH)
2Deng the surface deposition of meeting, thereby cause the heat exchanger heat transfer efficiency to reduce and cause underdeposit corrosion at pipeline and heat exchanger.
Because the shortage of water resources and the increase of process water expense, in order to save water coolant and to reduce blowdown flow rate, modern recirculated cooling water adopts methods such as adding water treatment agent to handle more, and cycles of concentration is controlled at 2.5～5.0 times operations usually.At this moment the scaling tendency of system increases, and equipment corrosion and microorganism growth also influence the safe operation of system simultaneously.Can solve or alleviate these problems by the way of adding water conditionings such as chemical agent, the most frequently used chemical agent has water conditioners such as dirt dispersion agent, inhibiter and biocide.
Anti-incrustation corrosion inhibitor has successively passed through inorganic anti-incrustation corrosion inhibitor, the stages such as natural polymer, polycarboxylate, organic phosphine class, multiple copolymer.But the mineral-type addition is big, and scale inhibition effect is relatively poor; Polycarboxylate and organic phosphine class functional group are more single; Multiple copolymer is few, the superior performance of add-on, advantage such as high temperature resistant then.And, medicament is required to want environmental protection, easily degraded along with environmental requirement improves, low to environmental influence.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can overcome that above-mentioned defective, production technique are simple, the methylene-succinic acid multi-component copolymer efficient scale inhibitor and the preparation method of no waste discharge.
Its concrete technical scheme is:
A kind of propenol itaconic acid sulfonate multipolymer scale inhibiting agent, it is characterized in that: be prepared from by methylene-succinic acid, sulfonate, vinylcarbinol aqueous polymerization under initiator system, with methylene-succinic acid weight is benchmark, the sulfonate add-on is 10%～50%, the vinylcarbinol add-on is 5%～20%, initiator content (is benchmark with the monomer mass) is 5%～30%, inferior sodium phosphate 5%～30%
Described propenol itaconic acid sulfonate multipolymer scale inhibiting agent, sulfonate is following one or more mixtures: propene sulfonic acid salt, vinyl sulfonate, styrene sulfonate etc., comparatively Shi Yi sulfonate is propene sulfonic acid salt, and add-on is 10%～50% (is benchmark with methylene-succinic acid weight).
Described propenol itaconic acid sulfonate multipolymer scale inhibiting agent, initiator comprises all initiators that can decompose under temperature of reaction of the present invention, the for example combination of following one or more oxygenants, or itself and single the kind or the combination of multiple reductive agent: Sodium Persulfate, ammonium persulphate, Potassium Persulphate, peroxophosphoric acid sodium, potassium superphosphate, ammonium superphosphate, hydrogen peroxide and tert-butyl peroxide, diacyl peroxide; Reductive agent is an inferior sodium phosphate, can join in the methylene-succinic acid solution before polymerization or even the adding in the reaction system in polymerization.With oxygenant or and the water-soluble respectively aqueous solution that is prepared into of reductive agent, form initiator system, its consumption is 5%～30% (is benchmark with the monomer mass), and configuration concentration is 5～30%, suitable oxygenant is a persulphate, can be mixedly configured into solution with 50% sulfonate.
The method for making of described propenol itaconic acid sulfonate multipolymer scale inhibiting agent, it is characterized in that adopting following steps: will be dissolved in water in methylene-succinic acid and sulfonate (50%) the adding reactor, with the methylene-succinic acid quality is benchmark, wherein the sulfonate add-on is 10%～50%, adding the water yield is 150%～500%, quantity of isopropanol is 40～80%, steady temperature is between 30～100 ℃, then add initiator solution with uniform feed rate, vinylcarbinol reacts in reactor, wherein active initiator content (is benchmark with the monomer mass) is 5%～30%, vinylcarbinol (is benchmark with the methylene-succinic acid quality) add-on is 5%～20%, is incubated 15～150 minutes again after adding material.
The method for making of described propenol itaconic acid sulfonate multipolymer scale inhibiting agent, the reinforced time of initiator and vinylcarbinol is 1～4 hour.
The method for making of described propenol itaconic acid sulfonate multipolymer scale inhibiting agent was reacted after adding material 15～150 minutes again.
The method for making of described propenol itaconic acid sulfonate multipolymer scale inhibiting agent, the reductive agent in the initiator join in the methylene-succinic acid solution before polymerization or evenly add in the reaction system in polymerization.
The finished product of the present invention are that solid content is 20%～40% (weight content) solution, but also are prepared into sheet or pulverulent solids behind the concentrate drying, or earlier with alkali such as sodium hydroxide, potassium hydroxide, ammonia neutralization, make solid again.
The present invention is raw material with the methylene-succinic acid, carries out the water copolymerization with vinylcarbinol, sulfonate, and more specifically saying so with the methylene-succinic acid is raw material, in the presence of initiator, carry out the aqueous free radical polymerization with vinylcarbinol, sulfonate, production technique is simple, and the product residual monomer is less, no waste discharge.The polymkeric substance that makes with this method is to the formation of dirts such as carbonate, Sulfates, phosphoric acid salt, silicates in cooling water system layer and be attached with restraining effect efficiently, and to ferric oxide, mud etc. play a good dispersion.
This polymkeric substance is good with water conditioner compatibleness commonly used, can with the composite uses of water conditioner such as organophosphate, zinc salt inhibiter, also can use separately, can under comparatively high temps, use, also can be used in the oil-field flooding as dirt dispersion agent.
This polymkeric substance is according to " the mensuration tosca method of water conditioner scale-inhibiting properties " GB/T 16632-2008, through the static-state scale inhibition experiment, compare superior performance with the Scale inhibitors that uses in the market such as hydrolytic polymaleic anhydride, 613, HEDP, ATMP, vinylformic acid-AMPS multiple copolymer etc.
The finished product of the present invention also can be used for scale remover, chelating, dispersion agent, washing auxiliary detergent etc.
Embodiment
Embodiment 1
In the four-hole boiling flask that mechanical stirrer, constant pressure funnel and thermometer are housed, add methylene-succinic acid 130g, Virahol 72g, distilled water 400g is heated to 60 ℃, and methylene-succinic acid is all dissolved; Sodium allylsulfonate 18g is dissolved in the 50g distilled water, after the methylene-succinic acid dissolving, adds fast; Be warmed up to 90 ℃ then; After being dissolved in sodium allylsulfonate 18g in the 55g distilled water, adding 100g distilled water and add 15g Sodium Persulfate preparation initiator again; Be mixed with reductive agent in 100g distilled water adding 27g inferior sodium phosphate and 15g vinylcarbinol; After methylene-succinic acid solution is warmed up to 70 ℃, add initiator 30ml and reductive agent 10ml earlier fast, in 2 hours, evenly be added dropwise in the beaker initiator, reductive agent, keep temperature of reaction at 90 ℃, after monomer and initiator dropwise, continue insulation (being incubated 20 minutes) reaction for some time (hereinafter to be referred as " reaction times ").Stop to heat, stirring, Virahol is reclaimed in distillation, and temperature is controlled at 101+2 ℃, adds liquid caustic soda, waits the interior temperature of four-hole boiling flask to drop to 75 ℃, adds the liquid caustic soda sodium, and cooling discharging gets the light tan thick liquid.
Chemical equation is as follows:
Resulting polymers solution transformation efficiency is 97.5% (is benchmark with the methylene-succinic acid), and unpolymerized remaining methylene-succinic acid monomer is 2.5%;
Resulting polymers density is 1.20g/cm3, and (25 ℃), solid content are 32.5%.
The test of resulting polymers scale inhibition performance (" the mensuration tosca method of water conditioner scale-inhibiting properties " GB/T16632-2008): contain Ca2+600mg/L, HC03-600mg/L, (in lime carbonate), under 80 ℃, constant temperature 10 hours, the medicine working concentration is 5mg/L (in a butt), keeps water sample pH ≈ 9.With calcium contents in the EDTA filtrates tested, test result is as follows:
Scale inhibitors kind resistance calcium carbonate scale rate
This polymkeric substance 68.97%
Hydrolytic polymaleic anhydride 40.5%
HEDP 52.29％
613 61.71％
ATMP 52.6％
Annotate: used hydrolytic polymaleic anhydride, 613, vinylformic acid-AMPS multiple copolymer, ATMP, HEDP are industrial goods in the experiment.
Embodiment 2
In the four-hole boiling flask that mechanical stirrer, constant pressure funnel and thermometer are housed, add methylene-succinic acid 150g, Virahol 72g, distilled water 400g is heated to 60 ℃, and methylene-succinic acid is all dissolved; Sodium allylsulfonate 8g is dissolved in the 50g distilled water, after the methylene-succinic acid dissolving, adds fast; Be warmed up to 90 ℃ then; After being dissolved in sodium allylsulfonate 8g in the 55g distilled water, adding 100g distilled water and add 8g Sodium Persulfate preparation initiator again; Be mixed with reductive agent in 100g distilled water adding 8g inferior sodium phosphate and 8g vinylcarbinol; After methylene-succinic acid solution is warmed up to 70 ℃, add initiator 30ml and reductive agent 10ml earlier fast, in 2 hours, evenly be added dropwise in the beaker initiator, reductive agent, keep temperature of reaction at 90 ℃, after monomer and initiator dropwise, continue insulation (being incubated 20 minutes) reaction for some time (hereinafter to be referred as " reaction times ").Stop to heat, stirring, Virahol is reclaimed in distillation, and temperature is controlled at 101 ± 2 ℃, adds liquid caustic soda, waits the interior temperature of four-hole boiling flask to drop to 75 ℃, adds the liquid caustic soda sodium, and cooling discharging gets the light tan thick liquid.
Resulting polymers solution transformation efficiency is 96.5% (is benchmark with the methylene-succinic acid), and unpolymerized remaining methylene-succinic acid monomer is 3.5%.Resulting polymers density is 1.19g/cm3 (25 ℃), and solid content is 29.8%.
Resulting polymers test scale inhibition performance is 51.8%.
Embodiment 3
In the four-hole boiling flask that mechanical stirrer, constant pressure funnel and thermometer are housed, add methylene-succinic acid 120g, Virahol 72g, distilled water 400g is heated to 60 ℃, and methylene-succinic acid is all dissolved; Sodium allylsulfonate 30g is dissolved in the 80g distilled water, after the methylene-succinic acid dissolving, adds fast; Be warmed up to 90 ℃ then; After being dissolved in sodium allylsulfonate 30g in the 100g distilled water, adding 100g distilled water and add 18g Sodium Persulfate preparation initiator again; Be mixed with reductive agent in 100g distilled water adding 36g inferior sodium phosphate and 24g vinylcarbinol; After methylene-succinic acid solution is warmed up to 70 ℃, add initiator 30ml and reductive agent 10ml earlier fast, in 2 hours, evenly be added dropwise in the beaker initiator, reductive agent, keep temperature of reaction at 90 ℃, after monomer and initiator dropwise, continue insulation (being incubated 20 minutes) reaction for some time (hereinafter to be referred as " reaction times ").Stop to heat, stirring, Virahol is reclaimed in distillation, and temperature is controlled at 101 ± 2 ℃, adds liquid caustic soda, waits the interior temperature of four-hole boiling flask to drop to 75 ℃, adds the liquid caustic soda sodium, and cooling discharging gets the light tan thick liquid.
Resulting polymers solution transformation efficiency is 98.9% (is benchmark with the methylene-succinic acid), and unpolymerized remaining methylene-succinic acid monomer is 1.1%.Resulting polymers density is 1.22g/cm3 (25 ℃), and solid content is 38.6%.
Resulting polymers test scale inhibition performance is 45.8%.
Claims (8)
1. propenol itaconic acid sulfonate multipolymer scale inhibiting agent, it is characterized in that, be prepared from by vinylcarbinol, methylene-succinic acid, sulfonate aqueous polymerization under initiator system, with the methylene-succinic acid quality is benchmark, the sulfonate add-on is 10%～50%, the vinylcarbinol add-on is 5%～20%, and initiator is 5%～30%, inferior sodium phosphate 5%～30%.
2. propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 1 is characterized in that, sulfonate is following one or more mixtures: propene sulfonic acid salt, styrene sulfonic acid salt, vinyl sulfonic acid salt.
3. propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 1, it is characterized in that initiator is selected from the combination of following wherein one or more and reductive agent: Sodium Persulfate, ammonium persulphate, Potassium Persulphate, peroxophosphoric acid sodium, potassium superphosphate, ammonium superphosphate, hydrogen peroxide, tert-butyl peroxide, diacyl peroxide; Reductive agent is an inferior sodium phosphate.
4. method for making for preparing as propenol itaconic acid sulfonate multipolymer scale inhibiting agent as described in the claim 1～3 is characterized in that adopting following steps:
(a) methylene-succinic acid and sulfonate being mixed and made into isopropanol water solution, is benchmark with the methylene-succinic acid quality, and the sulfonate add-on is 10%～50%, and quantity of isopropanol is 40～80%;
(b) add initiator solution, vinylcarbinol with uniform feed rate, wherein vinylcarbinol (is benchmark with the methylene-succinic acid quality) add-on is 5%～20%, and initiator content is that benchmark is 5%～30% with the monomer mass, inferior sodium phosphate 5%～30%;
(c) entire reaction course maintains the temperature at 60～102 ℃;
(d) reclaim Virahol, temperature is controlled at 101 ± 2 ℃;
(e) add the liquid caustic soda sodium, equitemperature drops to 75 ℃, adds the liquid caustic soda sodium, cooling discharging.
5. the method for making of propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 4, it is characterized in that: (a) to be mixed and made into the aqueous solution be to be dissolved in water by methylene-succinic acid and sulfonate for described methylene-succinic acid of step and sulfonate, and adding the water yield is 150%～500% of methylene-succinic acid quality.
6. the method for making of propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 4, it is characterized in that: the reinforced time of initiator and vinylcarbinol is 1～4 hour.
7. the method for making of propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 4 is characterized in that: (c) weigh step and reacted after adding material 15～150 minutes again.
8. the method for making of propenol itaconic acid sulfonate multipolymer scale inhibiting agent according to claim 4 is characterized in that: the reductive agent in the initiator joins in the methylene-succinic acid solution before polymerization or evenly adds in the reaction system in polymerization.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466814A (en) * | 2013-09-03 | 2013-12-25 | 山东天庆科技发展有限公司 | High temperature resisting composite water treatment agent and preparation method thereof |
| CN104445646A (en) * | 2014-11-25 | 2015-03-25 | 苏州佑君环境科技有限公司 | Scale removal and prevention agent for boiler and preparation method of scale removal and prevention agent |
| CN106345261A (en) * | 2016-08-23 | 2017-01-25 | 南京南炼宏泰技术开发有限公司 | Environmental-friendly high-efficacy deodorant and method for preparing same |
| CN114736325A (en) * | 2022-04-26 | 2022-07-12 | 山东泰和水处理科技股份有限公司 | Low-molecular-weight water-soluble 2-methallyl alcohol copolymer and preparation method and application thereof |
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| CN1511793A (en) * | 2002-12-29 | 2004-07-14 | 淄博矿业集团有限责任公司 | Polynary itaconic acid copolymer as high efficiency anti-sludging agent and preparing method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466814A (en) * | 2013-09-03 | 2013-12-25 | 山东天庆科技发展有限公司 | High temperature resisting composite water treatment agent and preparation method thereof |
| CN103466814B (en) * | 2013-09-03 | 2014-10-15 | 山东天庆科技发展有限公司 | High temperature resisting composite water treatment agent and preparation method thereof |
| CN104445646A (en) * | 2014-11-25 | 2015-03-25 | 苏州佑君环境科技有限公司 | Scale removal and prevention agent for boiler and preparation method of scale removal and prevention agent |
| CN106345261A (en) * | 2016-08-23 | 2017-01-25 | 南京南炼宏泰技术开发有限公司 | Environmental-friendly high-efficacy deodorant and method for preparing same |
| CN114736325A (en) * | 2022-04-26 | 2022-07-12 | 山东泰和水处理科技股份有限公司 | Low-molecular-weight water-soluble 2-methallyl alcohol copolymer and preparation method and application thereof |
| CN114736325B (en) * | 2022-04-26 | 2024-05-14 | 山东泰和科技股份有限公司 | Low molecular weight water-soluble 2-methylallyl alcohol copolymer and preparation method and application thereof |
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