CN101864047B - Ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor and preparation method thereof - Google Patents
Ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor and a preparation method thereof. The scale inhibitor is suitable for scale inhibition of calcium phosphate in a high-calcium high-pH industrial circulating cooling water system, is prepared by performing free radical polymerization reaction on a unsaturated double bond-containing carboxylic ester polyether monomer, an unsaturated carboxylic acid monomer, an unsaturated aromatic compound monomer, and has a structural general formula shown in the specifications, wherein E is a constitutional repeating unit after the unsaturated aromatic compound monomer is subjected to free radical polymerization reaction; R1 is -H or -COOH; R2, R3 and R4 are -H or C1-C4 low-carbon alkyl; R5 is one of C1-C4 low-carbon alkyl, -H, -SO3M, -CH2COOM, -CH(CH3)COOM, and -CH(CH2CH3)COOM; M is H<+>, K<+> or Na<+>; and the polymerization degree x is 1 to 5,000, the polymerization degree y is 1 to 5,000, the polymerization degree z is 1 to 5,000, and the polymerization degree n is 1 to 100.
Description
Technical field
The present invention relates to a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor and preparation method thereof, this Scale inhibitors is applicable to industrial circulating cooling water calcium phosphate scale inhibition, is particularly useful for the calcium phosphate scale inhibition of the high pH cooling water quality of high calcium, belongs to the Treatment of Industrial Water technical field.
Background technology
The calcium hardness great majority surpass 600mg/L (with CaCO in the underground water of domestic Central Plains, the Northwest and most of the Northeast and the minority surface water water
3Meter), total alkalinity surpasses 800mg/L (with CaCO
3Meter), belong to high rigidity high alkalinity water quality, very easily fouling.The outstanding problem of making the recirculated cooling water existence of this class water quality is the water cooler fouling, the water cooler that particularly heat exchanging intensity is large, flow velocity is less, and operation was stopped up because fouling causes water cooler less than the some months time continuously.Therefore, must be processed the good heat transfer effect of guarantee water cooler in long-term operation.The main employing in recirculating cooling water system added the phosphoric acid salt Scale inhibitors at present, such as hydroxy ethylene diphosphonic acid (HEDP), Amino Trimethylene Phosphonic Acid (AMP) and 2-phosphonic acids butane-1,2,4-tricarboxylic acid (PBTC) etc.But the biocide oxygenolysis that these phosphoric acid salt Scale inhibitorss are hydrolyzed or are existed in the system easily generates PO
4 3-Ion, through with water in the higher Ca of content
2+Effect generates polytype calcium phosphate precipitation, such as HPA[Ca
5(PO
4)
3OH], DCPD (CaHPO
42H
2O), OCP[Ca
4H (PO
4)
35H
2O], β-TCP[Ca
3(PO
4)
2], DCP (CaHPO
4) etc.The use of P containing sludge inhibitor easily makes bacterium algae amount reproduction and forms red tide and causes pollution to water surrounding in addition, so the use of research of non-phosphorus scale inhibitor more and more receives people's concern.At present the research of non-phosphorus scale inhibitor of excellent performance is the vinylformic acid-allyloxy polyethoxye co-polymer of sulfonate of U.S. Betz company, has excellent resistance calcium phosphate effect, but both there be not the fluorescent tracing group in its structure, there is not to measure with methods such as ultraviolets the phenyl ring group of its concentration yet, therefore can't realize on-line monitoring and automatic chemical feeding, easily cause the phenomenon of the untimely or polypharmacy of administration.The present invention utilizes the chelated calcium ability of the good water-soluble and carboxylic acid excellence of polyethers, carry out Raolical polymerizable with carboxylicesters polyether monomer, unsaturated carboxylic acid monomer, the unsaturated aromatics monomer that contains unsaturated double-bond, make a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor and preparation method thereof.In the ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor molecular structure that makes owing to contain the strong polyether group of wetting ability and the strong hydroxy-acid group of chelating calcium ability, so the scale inhibition to calcium phosphate in the industrial circulating cooling water system of the high pH of high calcium has efficient restraining effect, contain ultraviolet-labeled benzene ring structure in this Scale inhibitors molecular structure, ultraviolet-labeled method can be measured inhibitor concentration, to realize on-line monitoring and automatic chemical feeding function.
Technical scheme: a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of the present invention carries out Raolical polymerizable by the carboxylicesters polyether monomer that contains unsaturated double-bond, unsaturated carboxylic acid monomer, unsaturated aromatics monomer and gets, and its general structure is as follows:
Wherein: E is the repeated structural unit of unsaturated aromatics monomer after free-radical polymerized;
R1 is-H or-COOH; R2, R3 and R4 be-low-carbon alkyl of H or C1～C4; R5 be C1～C4 low-carbon alkyl ,-H ,-SO
3M ,-CH
2COOM ,-CH (CH
3) COOM ,-CH (CH
2CH
3) a kind of among the COOM, M is H
+Or K
+Or Na
+
Polymerization degree x is 1～5000, and polymerization degree y is 1～5000, and polymerization degree z is 1～5000, and polymerization degree n is 1～100.
The preparation method of above-mentioned a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor is:
At N
2Atmosphere, under the room temperature, the carboxylicesters polyether monomer that contains unsaturated double-bond of certain mass is added in the reactor, take the quality of the carboxylicesters polyether monomer that contains unsaturated double-bond as benchmark, add 0.1～2.0 times of distilled water that contains the carboxylicesters polyether monomer quality of unsaturated double-bond, mixing, after being warming up to 40～90 ℃, drip simultaneously inorganic initiator solution and mass percentage concentration the unsaturated aromatics aqueous solution as 5～80% of mass percentage concentration as 5～80% take uniform feed rate, mass percentage concentration is 5～80% the unsaturated carboxylic acid monomer aqueous solution; Take the quality of the carboxylicesters polyether monomer that contains unsaturated double-bond as benchmark, add-on without organic initiators is 0.01～0.5 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond, the add-on of unsaturated aromatics monomer is 0.1～20 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond, and the add-on of unsaturated carboxylic acid monomer or unsaturated carboxylic acid anhydride monomers is 0.1～20 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond; 0.5 after dropwising in～the 2.0h, continue reaction 0.5～5.0h, be down to room temperature, getting outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
Employed carboxylicesters polyether monomer is vinylformic acid carboxylicesters polyethers sulfonic acid among the preparation method of above-mentioned a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor, vinylformic acid carboxylicesters polyether sulfonate, vinylformic acid carboxylicesters polyether carboxylic acid, vinylformic acid carboxylicesters polyether carboxylation, methacrylic acid carboxylicesters polyethers sulfonic acid, methacrylic acid carboxylicesters polyether sulfonate, methacrylic acid carboxylicesters polyether carboxylic acid, methacrylic acid carboxylicesters polyether carboxylation, the vinylformic acid carboxylicesters polyethers of low-carbon alkyl end-blocking, the mixture of one or more in the methacrylic acid carboxylicesters polyethers of low-carbon alkyl end-blocking.
Employed unsaturated carboxylic acid monomer is one or more the mixture in vinylformic acid, methacrylic acid, methylene-succinic acid, toxilic acid, the maleic anhydride in the preparation process of above-mentioned a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor.
Employed unsaturated aromatics monomer is vinylbenzene, styrene sulfonate, 8-allyloxy-1 in the preparation process of above-mentioned a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor, 3,6-pyrene trisulfonate, 8-(4-vinyl benzyloxy base)-1, the mixture of one or more in 3, the 6-pyrene trisulfonate.
In the preparation process of above-mentioned a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor employed 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 mixture in the persulfonic acid sodium, persulfonic acid potassium, hydrogen peroxide.
Beneficial effect: a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of the present invention is to be carried out Raolical polymerizable and got by the carboxylicesters polyether monomer that contains unsaturated double-bond, unsaturated aromatics monomer, unsaturated carboxylic acid monomer, the eutrophy elements such as nonnitrogenous, phosphorus, polymerization process adopts " treating different things alike " mode, need not to separate environmental friendliness.In the ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor molecular structure that makes owing to contain the strong polyether group of wetting ability, so the scale inhibition to calcium phosphate in the industrial circulating cooling water system of the high pH of high calcium has efficient restraining effect, contain ultraviolet-labeled benzene ring structure in this Scale inhibitors molecular structure, can measure inhibitor concentration with ultraviolet-labeled method, to realize on-line monitoring and automatic chemical feeding function.
Embodiment
Example 1: at N
2Atmosphere, under the room temperature, be that 10 100g vinylformic acid carboxylicesters polyethers sodium sulfonate is dissolved in 150g distilled water with the polyethers polymerization degree n, mixing, after being warming up to 70 ℃, drip respectively simultaneously 33g maleic anhydride (being dissolved in 50g distilled water) with uniform feed rate, 33g Sodium styrene sulfonate (being dissolved in 50g distilled water), 7g Sodium Persulfate (being dissolved in 50g distilled water), temperature remains on 70 ℃ in the dropping process, after dropwising temperature is increased to 80 ℃ and continues insulated and stirred reaction 3h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1500mg/L, during pH=11.0, gained Scale inhibitors resistance calcium phosphate scale is 92.67%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.315.
Example 2: at N
2Atmosphere, under the room temperature, be that 20 200g vinylformic acid carboxylicesters polyether carboxylic acid sodium is dissolved in 150g distilled water with the polyethers polymerization degree n, mixing, after being warming up to 65 ℃, drip respectively simultaneously 100g vinylformic acid (being dissolved in 100g distilled water) with uniform feed rate, 50g Sodium styrene sulfonate (being dissolved in 50g distilled water), 10g persulfonic acid sodium (being dissolved in 80g distilled water), temperature remains on 65 ℃ in the dropping process, after dropwising temperature is increased to 80 ℃ and continues insulated and stirred reaction 3.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1750mg/L, during pH=11.0, gained Scale inhibitors resistance calcium phosphate scale is 89.35%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.229.
Example 3: at N
2Atmosphere, under the room temperature, be that 15 200g methacrylic acid carboxylicesters polyether carboxylic acid sodium is dissolved in 150g distilled water with the polyethers polymerization degree n, mixing, after being warming up to 75 ℃, drip respectively simultaneously 200g vinylformic acid (being dissolved in 100g distilled water) with uniform feed rate, 200g Sodium styrene sulfonate (being dissolved in 50g distilled water), 15g lays particular stress on-sulfinic acid potassium (being dissolved in 80g distilled water), temperature remains on 75 ℃ in the dropping process, after dropwising temperature is increased to 85 ℃ and continues insulated and stirred reaction 4.0h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1750mg/L, during pH=11.0, gained Scale inhibitors resistance calcium phosphate scale is 91.23%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.314.
Example 4: at N
2Atmosphere, under the room temperature, the vinylformic acid carboxylicesters polyethers that with the polyethers polymerization degree n is 7 200g methyl blocking is dissolved in 150g distilled water, mixing, after being warming up to 70 ℃, drip respectively simultaneously 150g methacrylic acid (being dissolved in 100g distilled water) with uniform feed rate, 200g 8-allyloxy-1,3,6-pyrene sodium trisulfonate (being dissolved in 50g distilled water), 15g Potassium Persulphate (being dissolved in 80g distilled water), temperature remains on 70 ℃ in the dropping process, after dropwising temperature is increased to 80 ℃ and continues insulated and stirred reaction 2.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1750mg/L, during pH=10.0, gained Scale inhibitors resistance calcium phosphate scale is 95.38%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.369.
Example 5: at N
2Atmosphere, under the room temperature, be that 5 150g methacrylic acid carboxylicesters polyethers sodium sulfonate is dissolved in 150g distilled water with the polyethers polymerization degree n, mixing, after being warming up to 75 ℃, drip respectively simultaneously 250g methacrylic acid (being dissolved in 100g distilled water) with uniform feed rate, 250g 8-allyloxy-1,3,6-pyrene sodium trisulfonate (being dissolved in 50g distilled water), 15g Potassium Persulphate (being dissolved in 80g distilled water), temperature remains on 75 ℃ in the dropping process, after dropwising temperature is increased to 80 ℃ and continues insulated and stirred reaction 3.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1250mg/L, during pH=9.0, gained Scale inhibitors resistance calcium phosphate scale is 88.32%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.397.
Example 6: at N
2Atmosphere, under the room temperature, be that 10 150g vinylformic acid carboxylicesters polyether carboxylic acid potassium is dissolved in 150g distilled water with the polyethers polymerization degree n, mixing, after being warming up to 78 ℃, drip respectively simultaneously 150g methylene-succinic acid (being dissolved in 100g distilled water) with uniform feed rate, 250g 8-allyloxy-1,3,6-pyrene sodium trisulfonate (being dissolved in 50g distilled water), 15g Potassium Persulphate (being dissolved in 80g distilled water), temperature remains on 75 ℃ in the dropping process, after dropwising temperature is increased to 85 ℃ and continues insulated and stirred reaction 3.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1250mg/L, during pH=10.0, gained Scale inhibitors resistance calcium phosphate scale is 89.64%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.358.
Example 7: at N
2Atmosphere, under the room temperature, the methacrylic acid carboxylicesters polyether carboxylic acid sodium that with the polyethers polymerization degree n is 10 150g ethyl capping is dissolved in 150g distilled water, mixing, after being warming up to 75 ℃, drip respectively simultaneously 400g maleic anhydride (being dissolved in 400g distilled water) with uniform feed rate, 50g 8-(4-vinyl benzyloxy base)-1,3,6-pyrene trisulfonic acid potassium (being dissolved in 50g distilled water), 15g hydrogen peroxide (being dissolved in 50g distilled water), temperature remains on 75 ℃ in the dropping process, after dropwising temperature is increased to 85 ℃ and continues insulated and stirred reaction 3.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1250mg/L, during pH=9.0, gained Scale inhibitors resistance calcium phosphate scale is 95.42%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.297.
Example 8: at N
2Atmosphere, under the room temperature, be that 10 100g vinylformic acid carboxylicesters polyether carboxylic acid's sodium and 100g vinylformic acid carboxylicesters polyethers sodium sulfonate mixing are dissolved in 150g distilled water with the polyethers polymerization degree n, after being warming up to 70 ℃, drip respectively simultaneously 150g methacrylic acid (being dissolved in 100g distilled water) with uniform feed rate, 200g 8-(4-vinyl benzyloxy base)-1,3,6-pyrene sodium trisulfonate (being dissolved in 50g distilled water), 15g Sodium Persulfate (being dissolved in 80g distilled water), temperature remains on 70 ℃ in the dropping process, after dropwising temperature is increased to 80 ℃ and continues insulated and stirred reaction 2.5h, after being down to room temperature, making outward appearance is a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
80 ℃ of gained scale inhibitor dosage 6mg/L, temperature, calcium ion concn is 1750mg/L, during pH=10.0, gained Scale inhibitors resistance calcium phosphate scale is 94.21%.When recording consumption and be 6mg/L with ultraviolet spectrophotometer (wavelength 223nm, 1cm cuvette), the absorbancy of Scale inhibitors is 0.357.
Claims (5)
1. ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor, it is characterized in that this Scale inhibitors carries out Raolical polymerizable by the carboxylicesters polyether monomer that contains unsaturated double-bond, unsaturated carboxylic acid monomer, unsaturated aromatics monomer and gets, its general structure is as follows:
Wherein: E is the repeated structural unit of unsaturated aromatics monomer after free-radical polymerized, unsaturated aromatics monomer is styrene sulfonate, 8-allyloxy-1,3,6-pyrene trisulfonate, 8-(4-vinyl benzyloxy base)-1, a kind of in 3, the 6-pyrene trisulfonate;
R1 is-H or-COOH; R2, R3 and R4 be-low-carbon alkyl of H or C1 ~ C4; R5 be C1 ~ C4 low-carbon alkyl ,-H ,-SO
3M ,-CH
2COOM ,-CH (CH
3) COOM ,-CH (CH
2CH
3) a kind of among the COOM, M is H
+Or K
+Or Na
+
Polymerization degree x is 1 ~ 5000, and polymerization degree y is 1 ~ 5000, and polymerization degree z is 1 ~ 5000, and polymerization degree n is 1 ~ 100.
2. the preparation method of a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor according to claim 1 is characterized in that the preparation method of this Scale inhibitors is:
At N
2Under atmosphere, the room temperature, the carboxylicesters polyether monomer that will contain unsaturated double-bond adds in the reactor, take the quality of the carboxylicesters polyether monomer that contains unsaturated double-bond as benchmark, add 0.1 ~ 2.0 times of distilled water that contains the carboxylicesters polyether monomer quality of unsaturated double-bond, mixing, after being warming up to 40～90 ℃, drip simultaneously the inorganic initiator solution of mass percentage concentration as 5～80%, the mass percentage concentration unsaturated aromatics aqueous solution and the unsaturated carboxylic acid monomer aqueous solution of mass percentage concentration as 5～80% as 5～80% take uniform feed rate; Take the quality of the carboxylicesters polyether monomer that contains unsaturated double-bond as benchmark, add-on without organic initiators is 0.01～0.5 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond, the add-on of unsaturated aromatics monomer is 0.1 ~ 20 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond, and the add-on of unsaturated carboxylic acid monomer is 0.1 ~ 20 times of quality that contains the carboxylicesters polyether monomer of unsaturated double-bond; 0.5 after dropwising in ~ the 2.0h, continue reaction 0.5～5.0h, be down to room temperature, getting outward appearance is the ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor of light yellow thick transparent liquid.
3. the preparation method of a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor according to claim 2, it is characterized in that the employed carboxylicesters polyether monomer that contains unsaturated double-bond is vinylformic acid carboxylicesters polyethers sulfonic acid among this preparation method, vinylformic acid carboxylicesters polyether sulfonate, vinylformic acid carboxylicesters polyether carboxylic acid, vinylformic acid carboxylicesters polyether carboxylation, methacrylic acid carboxylicesters polyethers sulfonic acid, methacrylic acid carboxylicesters polyether sulfonate, methacrylic acid carboxylicesters polyether carboxylic acid, methacrylic acid carboxylicesters polyether carboxylation, the vinylformic acid carboxylicesters polyethers of the low-carbon alkyl end-blocking of C1 ~ C4, the mixture of one or more in the methacrylic acid carboxylicesters polyethers of the low-carbon alkyl end-blocking of C1 ~ C4, wherein: vinylformic acid carboxylicesters polyether carboxylic acid, vinylformic acid carboxylicesters polyether carboxylation, methacrylic acid carboxylicesters polyether carboxylic acid, polyether carboxylic acid among the methacrylic acid carboxylicesters polyether carboxylation is polyethers acetic acid, the polyethers methyl acetic acid, a kind of in the polyethers ethyl acetic acid.
4. the preparation method of a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor according to claim 2 is characterized in that employed unsaturated carboxylic acid monomer among this preparation method is one or more the mixture in vinylformic acid, methacrylic acid, the toxilic acid.
5. the preparation method of a kind of ultraviolet-labeled high-calcium-resistant high-pH scale inhibitor according to claim 2 is characterized in that employed among this preparation method is one or more mixture in Sodium Persulfate, Potassium Persulphate, persulfonic acid sodium, persulfonic acid potassium, the hydrogen peroxide without organic initiators.
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| 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 |
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