循环冷却系统污垢中无机磷提取方法优化

doi:10.11949/j.issn.0438-1157.20181016

摘要/Abstract

摘要：

再生水中磷绝大部分为无机磷，是引起循环冷却系统结垢腐蚀的重要因素。为了探究无机磷在系统内的迁移转化及其对系统的影响，无机磷的定量定性尤为重要。在分析了无机磷的SMT( standard measurements and testing)连续提取法在循环冷却系统污垢提取中应用的可行性的基础上，对SMT提取方法进行条件优化，建立了污垢中无机磷定性定量分析方法。结果表明，优化后的SMT连续提取法能够实现对系统内污垢中无机磷的完全提取，且回收率接近100%；污垢中弱吸附态磷（NH₄Cl-P）、铝结合态磷（Al-P）、铁结合态磷（Fe-P）和钙结合态磷（Ca-P）4种形态无机磷能得到完全分离。

关键词: 循环冷却水系统, 无机磷, 结垢, 腐蚀, SMT连续提取法

Abstract:

Most of the phosphorus in the reclaimed water is inorganic phosphorus, which is an important factor causing scale corrosion of the circulating cooling system. To explore the migration and transformation of inorganic phosphorus in the system and its influence on the system, the quantitative determination of inorganic phosphorus is particularly important. The feasibility of SMT continuous extraction of inorganic phosphorus in the fouling of the circulating cooling system was carried out, the inorganic phosphorus SMT was optimized and improved, and a qualitative and quantitative analysis method for inorganic phosphorus was established. The results showed that the majorization of SMT extraction method was able to extract the inorganic phosphorus in the scale completely, the recovery rate was close to 100%， and weakly adsorbed phosphorus (NH₄Cl-P), aluminum-bound phosphorus (Al-P), iron-bound phosphorus (Fe-P) and calcium-bound phosphorus (Ca-P) in the scale can be completely separated.

Key words: circulating cooling water system, inorganic phosphorus, scaling, corrosion, SMT extraction method

中图分类号:

X 703.1

张玉玲, 张利平, 王倩, 李旭东, 刘晓冬, 张敬红. 循环冷却系统污垢中无机磷提取方法优化[J]. 化工学报, 2019, 70(3): 1083-1088.

Yuling ZHANG, Liping ZHANG, Qian WANG, Xudong LI, Xiaodong LIU, Jinghong ZHANG. Optimization of extraction process of inorganic phosphorus in scale of circulating cooling system[J]. CIESC Journal, 2019, 70(3): 1083-1088.

图/表 8

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无机磷形态	提取方法
弱吸附态磷（NH₄Cl-P）	1 mol/L NH₄Cl溶液，振荡离心，过滤，测定提取液中磷浓度
铝结合态磷（Al-P）	0.5 mol/L NH₄F溶液（pH 8.2），振荡，离心，过滤，测定提取液中磷浓度
铁结合态磷（Fe-P）	0.1 mol/L NaOH、0.5 mol/L Na₂CO₃混合提取液振荡提取，离心，过滤，向提取液中加入1 ml浓硫酸，测定磷浓度
钙结合态磷（Ca-P）	1 mol/L H₂SO₄振荡1h，离心，过滤，调pH至中性，测定提取液中磷浓度
残渣磷（Res-P）	残渣550℃灼烧5 h，1 mol/L HCl，振荡，离心，过滤，测定提取液中磷浓度

无机磷形态	提取方法
弱吸附态磷（NH₄Cl-P）	1 mol/L NH₄Cl溶液，振荡离心，过滤，测定提取液中磷浓度
铝结合态磷（Al-P）	0.5 mol/L NH₄F溶液（pH 8.2），振荡，离心，过滤，测定提取液中磷浓度
铁结合态磷（Fe-P）	0.1 mol/L NaOH、0.5 mol/L Na₂CO₃混合提取液振荡提取，离心，过滤，向提取液中加入1 ml浓硫酸，测定磷浓度
钙结合态磷（Ca-P）	1 mol/L H₂SO₄振荡1h，离心，过滤，调pH至中性，测定提取液中磷浓度
残渣磷（Res-P）	残渣550℃灼烧5 h，1 mol/L HCl，振荡，离心，过滤，测定提取液中磷浓度

样品编号	沉积物质量/g	理论含磷量/mg	回收磷量/mg	回收率/%
1	5.1354	258.10	259.73	100.63
2	5.1363	260.42	252.92	97.12
3	5.1691	260.59	262.41	100.70
4	4.1339	258.20	251.64	97.46

样品编号	沉积物质量/g	理论含磷量/mg	回收磷量/mg	回收率/%
1	5.1354	258.10	259.73	100.63
2	5.1363	260.42	252.92	97.12
3	5.1691	260.59	262.41	100.70
4	4.1339	258.20	251.64	97.46

Sample serial number	NH₄Cl-P (mg/g)	Al-P (mg/g)		Fe-P (mg/g)	Ca-P (mg/g)	Total particulate inorganic phosphorus/mg	Total dissolved inorganic phosphorus/mg	Experimentally measured inorganic phosphorus /mg	Inorganic phosphorus addition/mg	Recovery rate/%
1	1.598	1.54		0.826	2.98	1016.06	55.74	1061.80	1061.58	100.96
1	1.592	1.548		0.822	3.08	1009.58	55.74	1062.32	1061.58	100.35
2	1.552		2.392	0.634	1.78	1032.98	15.94	1048.92	1062.16	98.75
2	1.566		2.412	0.586	1.792	1024.60	15.94	1040.54	1062.16	97.96
3	1.356		2.208	1.116	1.476	997.80	31.11	1028.91	1062.81	96.81
3	1.372		2.17	1.13	1.488	1024.32	31.11	1055.42	1062.81	99.30