CN102786156A - Sulfonic acid group-containing attapulgite corrosion and scale inhibitor and preparation method as well as application thereof - Google Patents
Sulfonic acid group-containing attapulgite corrosion and scale inhibitor and preparation method as well as application thereof Download PDFInfo
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- CN102786156A CN102786156A CN2012102929136A CN201210292913A CN102786156A CN 102786156 A CN102786156 A CN 102786156A CN 2012102929136 A CN2012102929136 A CN 2012102929136A CN 201210292913 A CN201210292913 A CN 201210292913A CN 102786156 A CN102786156 A CN 102786156A
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Abstract
The invention discloses a sulfonic acid group-containing attapulgite corrosion and scale inhibitor and a preparation method as well as application thereof, and belongs to the technical field of water treatment. The preparation method of the sulfonic acid group-containing attapulgite corrosion and scale inhibitor comprises the following steps of: dissolving attapulgite in water; raising temperature; dropwise adding saturated aqueous solution of sodium p-styrene sulfonate and maleic anhydride into an attapulgite water system; dropwise adding ammonium persulfate aqueous solution serving as an initiator in 10-15 minutes; and stirring at a constant temperature and then performing evaporative crystallization to prepare the sulfonic acid group-containing attapulgite corrosion and scale inhibitor. The environment-friendly scale inhibitor synthesized by the invention has the advantages of wide raw material source, good water solubility, no secondary pollution caused to water, good tolerance to Ca<2+>, excellent scale inhibition effect on calcium carbonate and good ferric oxide dispersion effect. The preparation method has the advantages of cheap, simple and readily available raw materials, simple synthetic line and low reaction condition requirements; and the synthesized scale inhibitor has the advantages of good water solubility, good calcium carbonate scale inhibition and good ferric oxide dispersion performance.
Description
Technical field
The invention belongs to water-treatment technology field, relate to the water treatment scale agent, particularly a kind of sulfonic group attapulgite corrosion inhibiting and descaling agent that contains.
Background technology
Shortage of water resources is the severe problem that the China and even the whole world all will face, and China is one of serious country of shortage of water resources, in today of water resources growing tension, improves industrial cooling water efficient, can effectively reduce the water resources demand, alleviates water resources pressure.The efficient of raising industrial cooling water the most effectively one of way is the recycling of recirculated cooling water; But the serious problem that the recycling recirculated cooling water can bring; It is exactly the accumulation of salinity; And the accumulation of salinity can bring the fouling and the etching problem of heat-exchange equipment, and developing good corrosion inhibiting and descaling agent is the good way that addresses this problem.At present corrosion inhibiting and descaling agent commonly used is main with phosphorus system in the industry, but it can cause the eutrophication of water body after water-soluble, and therefore novel non-phosphorus scale agent is present research focus, and sulphonate receives extensive concern because of its good scale inhibition effect.
The resource reserve of China's attapulgite is very big; Because that finds is later, its deep development utilizes level lower, in addition a little less than the relative thin of China's nonmetalliferous ore processing industry basis; The kind of the attapulgite products that can produce is compared considerably less with other country; The application of the mineral reserve that this economic implications is great also is only limited to general filler production, even with the cheap outlet of the form of original soil, has caused the waste of resource.Now, attapulgite is applied to the processing of waste water from dyestuff and the preparation of various water conditioners gradually with its good adsorptivity, but rarely has the report about its Scale inhibitors aspect at present.Therefore, utilize the resourceful characteristics of China's attapulgite, develop usury, be significant for the development research of this Mineral resources with the product that is worth.Particularly improve its compactness, thereby develop the higher green compound type Scale inhibitors of scale-inhibiting properties, also help to satisfy the needs that China's process water is handled through modification.
(1) the building materials world, 2010,31 (3): 7-9, reported that with methylpropene sodium sulfonate, vinylformic acid, acrylic amide be monomer, in water, be initiator with the ammonium persulphate, Virahol is a synthetic copolymer under the condition of chain transfer base; This polymkeric substance has good scale inhibition effect to lime carbonate, but works as Ca
2+When concentration reached 500 mg/ L, scale inhibition performance had only 57. 8%, was not very high to the tolerance of calcium ion; And used Virahol in the experiment; Virahol is poisonous, eats or suck symptoms such as a large amount of steams can cause flushing, headache, spirit depressing, feels sick, stupor, is discharged in the water; Not only bring environmental pollution, also can damage human body;
(2) Desalination 2009,249:1-4, and having introduced with maleic anhydride (MA), SSS (SS) is monomer; Hypophosporous Acid, 50 and hydrogen peroxide are initiator; Obtained a kind of novel Scale inhibitors, this initiator has good scale inhibition effect, but has used Hypophosporous Acid, 50 in its initiator; Can cause the eutrophication of water body after water-soluble, cause environmental pollution;
(3) Yunnan chemical, 2011,38 (5): 1-6; Having introduced with HPMA (HPMA), poly-epoxy succinic acid (PESA), Sunmorl N 60S, sodium D-isoascorbate and zinc salt is raw material; Develop a kind of novel non-phosphate corrosion inhibiting and descaling agent, experiment shows that changing Scale inhibitors has good scale inhibition effect and corrosion mitigating effect, but its raw material is complicated; And introduced zinc salt, may cause secondary pollution.
Summary of the invention
To the extensive storage capacity of attapulgite and good water treatment effect thereof, and the deficiency that exists in the above-mentioned preparation process, the invention discloses a kind of preparation method who contains sulfonic group novel green Scale inhibitors.
A kind of preparation method who contains sulfonic group attapulgite corrosion inhibiting and descaling agent; Be earlier attapulgite to be dissolved in the water, heat up, be added drop-wise in the attapulgite aqueous systems with sodium p styrene sulfonate with the saturated aqueous solution of maleic anhydride then; Again the initiator ammonium persulfate aqueous solution is dropwised in 10 ~ 15min; Constant temperature stirs the back evaporative crystallization, makes to form
Described attapulgite quality accounts for 1% ~ 25%, preferred 10% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described sodium p styrene sulfonate quality accounts for 15% ~ 80%, preferred 65% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described maleic anhydride quality accounts for 0.7% ~ 30%, preferred 25% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described initiator ammonium persulfate accounts for 5% ~ 15%, preferred 8% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described intensification reaches 50 ℃ ~ 90 ℃, preferred 70 ℃.
Beneficial effect
Advantage of the present invention: (1) cost of material is cheap, be simple and easy to; (2) synthetic route is simple, and synthesis condition requires lower; (3) the synthetic Scale inhibitors has good water-solubility; (4) have good resistance calcium carbonate scale and dispersing iron oxide performance.The present invention has synthesized the environmental friendliness green scale inhibitor, and this polymkeric substance not only raw material sources is extensive, has good water-solubility, and can not cause secondary pollution to water body.To Ca
2+Tolerance good, lime carbonate is had good scale inhibition effect, good dispersing iron oxide effect is arranged again simultaneously.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
Take by weighing 0.2g attapulgite (ATT) and add in the four-hole boiling flask, add an amount of zero(ppm) water, start stirring and be heated to 80 ℃; Take by weighing 3g sodium p styrene sulfonate (SSS) and 1g maleic anhydride (MA), make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 12% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 5h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-1).The resistance calcium carbonate scale rate of gained ATP-1 is 86.83%, and the transmittance of dispersing iron oxide is 80.0%.
Embodiment 2
The attapulgite (ATT) that takes by weighing 1g adds in the four-hole boiling flask, adds an amount of zero(ppm) water, starts stirring and is heated to 70 ℃; Take by weighing the sodium p styrene sulfonate (SSS) of 2.5g and the maleic anhydride (MA) of 0.8g, make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 10% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 5h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-2).The resistance calcium carbonate scale rate of gained ATP-2 is 88.02%, and the transmittance of dispersing iron oxide is 76.4%.
Embodiment 3
The attapulgite (ATT) that takes by weighing 0.6g adds in the four-hole boiling flask, adds an amount of zero(ppm) water, starts stirring and is heated to 50 ℃; Take by weighing the sodium p styrene sulfonate (SSS) of 4g and the maleic anhydride (MA) of 1g, make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 12% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 4h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-3).The resistance calcium carbonate scale rate of gained ATP-3 is 91.31%, and the transmittance of dispersing iron oxide is 74.7%.
Embodiment 4
The attapulgite (ATT) that takes by weighing 0.6g adds in the four-hole boiling flask, adds an amount of zero(ppm) water, starts stirring and is heated to 90 ℃; Take by weighing the sodium p styrene sulfonate (SSS) of 2.5g and the maleic anhydride (MA) of 0.8g, make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 8% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 2h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-4).The resistance calcium carbonate scale rate of gained ATP-4 is 90.70%, and the transmittance of dispersing iron oxide is 72.4%.
Embodiment 5
The attapulgite (ATT) that takes by weighing 0.6g adds in the four-hole boiling flask, adds an amount of zero(ppm) water, starts stirring and is heated to 70 ℃; Take by weighing the sodium p styrene sulfonate (SSS) of 2.5g and the maleic anhydride (MA) of 0.8g, make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 10% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 6h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-5).The resistance calcium carbonate scale rate of gained ATP-5 is 95.42%, and the transmittance of dispersing iron oxide is 81.4%.
Embodiment 6
The attapulgite (ATT) that takes by weighing 0.6g adds in the four-hole boiling flask, adds an amount of zero(ppm) water, starts stirring and is heated to 80 ℃; Take by weighing the sodium p styrene sulfonate (SSS) of 2.5g and the maleic anhydride (MA) of 0.8g, make its dissolving, and it is added in the pyriform funnel with an amount of zero(ppm) water; Take by weighing 8% initiator ammonium persulfate (NH
4)
2S
2O
8, with an amount of zero(ppm) water it is dissolved, join in another pyriform funnel; In another mouthful of four-hole boiling flask, insert TM, treat that attapulgite disperses fully after, begin to drip respectively the mixed solution of initiator and SSS/MA; SSS/MA drips at the fixed time, and initiator adds the about 10 ~ 15min in back at SSS/MA and adds, and constant temperature stirs 4h then, will react the crystallization of gained solution evaporation, obtains green scale inhibitor (ATP-6).The resistance calcium carbonate scale rate of gained ATP-6 is 98.11%, and the transmittance of dispersing iron oxide is 64.0%.
Table 1 has been listed the performance of Scale inhibitors, and the synthesis condition that demonstrates Scale inhibitors is simple, to Ca
2+Good tolerance is arranged, scale inhibition performance and dispersing iron oxide efficient are preferably arranged.
Table 1
| Temperature of reaction (℃) | 70 |
| Reaction times (h) | 4 |
| C(Ca 2+Scale inhibition performance during)=500mg/L (%) | 85.17 |
| The highest scale inhibition performance (%) | 99.02 |
| Optimal decentralized red stone transmittance (%) | 64.0 |
The result shows that the present invention has synthesized the environmental friendliness green scale inhibitor, and this polymkeric substance not only raw material sources is extensive, has good water-solubility, and can not cause secondary pollution to water body.To Ca
2+Tolerance good, lime carbonate is had good scale inhibition effect, good dispersing iron oxide effect is arranged again simultaneously.
Claims (4)
1. preparation method who contains sulfonic group attapulgite corrosion inhibiting and descaling agent; Be earlier attapulgite to be dissolved in the water, heat up, be added drop-wise in the attapulgite aqueous systems after with sodium p styrene sulfonate with maleic anhydride then with water dissolution; Again the initiator ammonium persulfate aqueous solution is dropwised in 10 ~ 15min; Constant temperature stirs the back evaporative crystallization, makes to form, and it is characterized in that:
Described attapulgite quality accounts for 1% ~ 25%, preferred 10% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described sodium p styrene sulfonate quality accounts for 15% ~ 80%, preferred 65% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described maleic anhydride quality accounts for 0.7% ~ 30%, preferred 25% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction;
Described initiator ammonium persulfate accounts for 5% ~ 15%, preferred 8% of attapulgite, sodium p styrene sulfonate and the maleic anhydride quality sum of participating in reaction.
2. the preparation method who contains sulfonic group attapulgite corrosion inhibiting and descaling agent according to claim 1 is characterized in that, described intensification reaches 50 ℃ ~ 90 ℃, preferred 70 ℃.
3. the said preparation method of claim 1 prepares contains sulfonic group attapulgite corrosion inhibiting and descaling agent.
4. claim 3 is prepared contains the application of sulfonic group attapulgite corrosion inhibiting and descaling agent as Scale inhibitors.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242091A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of water process corrosion inhibiting and descaling agent and its preparation method and application |
| CN106242090A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of phosphate-free corrosion inhibition antisludging agent and its preparation method and application |
| CN106630270A (en) * | 2016-12-06 | 2017-05-10 | 福建海西滤水龙头研究中心有限公司 | Anti-scaling multi-membrane filtration compound filter element and filtering faucet |
| CN111003820A (en) * | 2019-12-27 | 2020-04-14 | 东北石油大学 | Solid slow-release scale inhibitor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101779654A (en) * | 2009-12-21 | 2010-07-21 | 许庆华 | Attapulgite oil-extracting and water-injecting sterilizing algicide for oil field |
| CN102504099A (en) * | 2011-11-17 | 2012-06-20 | 盐城纺织职业技术学院 | Preparation method for modified maleic anhydride-styrene sodium sulfonate copolymer serving as antibacterial scale inhibitor |
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2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101779654A (en) * | 2009-12-21 | 2010-07-21 | 许庆华 | Attapulgite oil-extracting and water-injecting sterilizing algicide for oil field |
| CN102504099A (en) * | 2011-11-17 | 2012-06-20 | 盐城纺织职业技术学院 | Preparation method for modified maleic anhydride-styrene sodium sulfonate copolymer serving as antibacterial scale inhibitor |
Non-Patent Citations (2)
| Title |
|---|
| HAN HONG等: "Applied Study on Composite Type of Industrial Corrosion and Scale Inhibitor Preparation with Hot Acid Treated Attapulgite Clay", 《CDCIEM"11 PROCEEDING OF THE 2011 INTERNATIONAL CONFERENCE ON COMPUTER DISTRIBUTED CONTROL AND INTELLIGENT ENVIRONMENTAL MONITORING》 * |
| 周玲: "磺化苯乙烯-马来酸酐共聚物的合成及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242091A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of water process corrosion inhibiting and descaling agent and its preparation method and application |
| CN106242090A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of phosphate-free corrosion inhibition antisludging agent and its preparation method and application |
| CN106630270A (en) * | 2016-12-06 | 2017-05-10 | 福建海西滤水龙头研究中心有限公司 | Anti-scaling multi-membrane filtration compound filter element and filtering faucet |
| CN111003820A (en) * | 2019-12-27 | 2020-04-14 | 东北石油大学 | Solid slow-release scale inhibitor and preparation method thereof |
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Application publication date: 20121121 |