高纯度气体二氧化氯生成反应动力学及其对微生物的杀菌研究
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摘要
研究针对微生物的高效杀菌剂是遏制生物武器杀伤威力的有效对策。气体ClO_2因具有优异的高效广谱杀菌性能且有毒副产物含量较低而倍受青睐。本文从高纯度气体ClO_2的生成方法、反应动力学以及ClO_2对微生物的杀菌效果等方面进行了研究。
(1)高纯度气体ClO_2生成技术及ClO_2浓度、纯度检测技术研究
提出了NaClO_3—NaClO_2组合法生成高纯度气体ClO_2的新工艺。HCl与NaClO_3在主反应器内反应，生成的Cl_2和ClO_2混合气体通过NaClO_2的固定床，将Cl_2进一步转化为ClO_2气体，最终产物气中ClO_2／Cl_2≈60／1，ClO_2纯度达到98．19％。制备了快速测试ClO_2浓度的标准比色卡及配套测试卡，所得测试卡测试ClO_2溶液浓度的范围为5～1000mg／L，测试误差在10％以内。
(2)高纯度气体ClO_2反应动力学研究
提出了HCl与NaClO_3反应可能存在的假设机理，并进行了验证。通过理论上对亚氯酸钠与氯气发生气固反应的微观分析，建立了NaClO_2与Cl_2发生气固反应的固定床——等效粒子模型并进行表征，得出了NaClO_3—NaClO_2组合工艺生成高纯度气体ClO_2的反应动力学模型。
(3)气体二氧化氯爆炸特性和爆炸机理研究
首次在20L的柱状爆炸罐内研究了气体ClO_2的爆炸特性，考查了气体ClO_2的爆炸极限及浓度对爆炸压力、爆炸诱导时间的影响。得出了气体ClO_2的爆炸下限为9．5％(体积比)，爆炸上限为100％；气体ClO_2的爆炸压力随浓度的增加而增大，最大爆炸压力出现的诱导时间随着气体ClO_2浓度的增加而缩短。提出了气体ClO_2的爆炸属于分解爆炸，其爆炸机理是涉及到中间稳定物——Cl_2O_3的特殊衰减支链分解爆炸机理，Cl_2O_3是引发、促进支链反应的主要因素。
(4)高纯度气体ClO_2生成系统装置研究
利用安全原理设计了高纯气体ClO_2反应器，ClO_2发生量达到了1．5kg／次以上，NaClO_2转化率达到93．7％、NaClO_3转化率达到95．5％时，气体ClO_2的产率最高达到97．3％，纯度达到了98．55％以上。NaClO_3—NaClO_2组合工艺生成高纯度的气体ClO_2，控制反应时间在30～45min左右较好。理论产量与实际产量二者的偏差在6．2％以内；超出此时间范围，实际产量与动力学计算结果的偏差会越来越大。
(5)气体ClO_2的应用研究
a高纯度气体ClO_2对葡萄的杀菌保鲜研究
研究了气体ClO_2对葡萄表面致病菌——葡萄球菌、大肠杆菌、李斯特单增菌和腐生酵母菌的杀菌效果。得出了气体ClO_2浓度增加和杀菌时间的延长，可以使杀菌效果很快的提高，在气体ClO_2杀菌浓度为25mg/L、杀菌时间12min、杀菌温度25℃的较佳条件下，金黄色葡萄球菌、李斯特单增菌和腐生酵母菌均减少了6．4log量级以上，而大肠杆菌达到5．76log量级。ClO_2的作用浓度和杀菌时间存在协同增效的作用。气体ClO_2对葡萄的保鲜效果研究表明，常温下采用浓度为30ml／m~3的气体ClO_2处理葡萄效果最好。ClO_2可以迅速有效地阻止蛋氨酸的分解，消除乙烯等物质并杀灭腐败菌，从而延缓果蔬变质过程，减少营养成分损失，起到长期保鲜的作用。
b二氧化氯消毒城市生活废水研究
研究表明，污水中粪大肠菌的灭菌效果随着ClO_2浓度和作用时间的增加而增加，得出了ClO_2消毒城市污水的投药浓度为5 mg／L、杀菌时间为20min的最佳条件，粪大肠菌杀菌率达到99．99％的去除率极限。处理后的出水中未检出CHCl_3，CCl_4的含量虽然随ClO_2浓度不同而有所区别，但是含量很少且差别不大。研究结果证实ClO_2消毒水体形成卤代烃类明显低于普通含氯消毒剂，将ClO_2用于污水消毒增强了回用污水的环境安全性。
It is the most effective countermove to exploit the highly active germicidal agentagainst the lethality of biological weapon.ClO_2 gas has attracted attention in the views ofbroad spectrum and highly active bactericidal ability and few or none poisonous byproducts.In this paper,the formative technology of high-purity ClO_2 gas,kinetics of its reaction andbactericidal effect were studied.
(1) Study on the generation of high-purity ClO_2 gas and the determination of itsconcentration and purity
A new technology used the NaClO_3-NaClO_2 compound mode to generated ClO_2 gas wasset forth.The reaction of HCl and NaClO_3 was proceed in main reactor,and,the generatedgaseous mixture containing Cl_2 and ClO_2 enter into the fixed bed reactor loaded NaClO_2granule,where Cl_2 was inverted into ClO_2,and the ClO_2/Cl_2 is 60/1 approximately in the endproducts,the purity of ClO_2 was up to 98.19%.The colorimetric card and test cardcorresponding to concentration of ClO_2 rapid determination were prepared,and the errorpercentage was less than 10% in test specification 5～1000mg/L.
(2) The kinetics of the formation reaction of high-purity ClO_2 gas
The mechanics hypothesis about chemical reaction of HCl and NaClO_3 was set forth,andbeen verified furtherly.The fixed bed and equivalent particle model was established bymicrostructure analysis of gas-solid reaction of NaClO_2 and Cl_2,and the reaction kineticsmodel,using NaClO_3-NaClO_2 compound technology to generate high-purity ClO_2 gas wasobtained.
(3) The explosion characteristics and mechanics of ClO_2 gas
It was the first time for the explosion characteristics of ClO_2 gas was studied in acylindrical exploder with a shell capacity of 20 liters.The impact of concentration toexplosion limit,explosion pressure and induction time were determinated.The experimentalresults indicated that the lower concentration limit for the explosive decomposition ofchlorine dioxide gas was 9.5% ([ClO_2]/[air]),the upper concentration limit was 100%,and thepressure of explosion increased with increasing concentration of ClO_2 gas,the induction time(the time from the moment of sparking to explosion) to attain the maximum pressure of explosion was shorten with increasing concentration of ClO_2 gas.The explosion reaction styleof ClO_2 is decomposition,the reaction mechanism of ClO_2 is of a degenerate chain-branchingtype involving the formation of a stable intermediate Cl_2O_3,and it is the major factor toinitiating and accelerating branched chain reaction.
(4) System device for generating high-purity ClO_2 gas
Following the principle of safety,the reactor to generated high-purity ClO_2 gas wasprepared.The production capacity of ClO_2 gas attained 1.5kg/batch,the percent conversion ofNaClO_2 and NaClO_3 were up to 93.7% and 95.5% respectively,the productive rate of ClO_2gas attained 97.3%,its purity was more than 98.55%.The optimum reaction time range wasfrom 30 to 45 minutes,the deviation of ClO_2 yield between theoretically,and,actually,was nomore than 6.2%,but the deviation of actual output to computing result by dynamics methodbecame more and more when the reaction time exceed the optimum range.
(5) Research on the application of ClO_2 gas
a Effect of ClO_2 gas on bactericidal and keep fresh on grape
The regularity of sterilization to Staphylococcus Aureus,Escherichia Coli 0157.H7,Listeria Monocytogenes and Saprophytic Yeast on grape surface with ClO_2 gas were studiedin this paper.The result showed that the bactericidal effect was markedly increased alongwith the concentration increased of ClO_2 gas and the bactericidal time in the experiment range.When the ClO_2 gas concentration 25mgl~(-1),bactericidal time 12min and temperature 25℃,Staphylococcus Aureus,Listeria Monocytogenes and Saprophytic Yeast decreased more than6.41og,but the decrease of Escherichia Coli 0157:H7 attained 5.761og.There exist synergismeffect between the bactericidal time and ClO_2 concentration.The result also showed that itwas best condition for grape to keep fresh when the concentration of ClO_2 gas is 30ml/m~3,ClO_2 gas can inhibit effectively methionine catabolic process decrease,the generating ofethene when killing the Saprospira on the surface of fruit and vegetable,so it is useful todelay metamorphic process,reduce nutritional ingredient loss,and keep the fruit andvegetable fresh for a long time.
b The municipal wastewater disposal by ClO_2
The result showed that the sterilizing effect to bacillus coli was increasing with theconcentration of ClO_2 and the treating duration increasing,the optimum were ClO_2concentration 5mg/L and bactericidal time 20min,the bactericidal ratio to bacillus coli was99.99%,which is limit bactericidal limit.After wastewater disposal,the CHCl_3 had not been detected in the water,the content of ClC_4 existed difference in some degree with the differentClO_2 concentration,but the real content is lower.The results indicate that the content ofhalogenated hydrocarbon are less than other common chlorine disinfectors after wastewaterare disposed by ClO_2,therefore,environment security is enhanced by using the ClO_2 gas tosterilized recycle-water.
(1)高纯度气体ClO_2生成技术及ClO_2浓度、纯度检测技术研究
提出了NaClO_3—NaClO_2组合法生成高纯度气体ClO_2的新工艺。HCl与NaClO_3在主反应器内反应，生成的Cl_2和ClO_2混合气体通过NaClO_2的固定床，将Cl_2进一步转化为ClO_2气体，最终产物气中ClO_2／Cl_2≈60／1，ClO_2纯度达到98．19％。制备了快速测试ClO_2浓度的标准比色卡及配套测试卡，所得测试卡测试ClO_2溶液浓度的范围为5～1000mg／L，测试误差在10％以内。
(2)高纯度气体ClO_2反应动力学研究
提出了HCl与NaClO_3反应可能存在的假设机理，并进行了验证。通过理论上对亚氯酸钠与氯气发生气固反应的微观分析，建立了NaClO_2与Cl_2发生气固反应的固定床——等效粒子模型并进行表征，得出了NaClO_3—NaClO_2组合工艺生成高纯度气体ClO_2的反应动力学模型。
(3)气体二氧化氯爆炸特性和爆炸机理研究
首次在20L的柱状爆炸罐内研究了气体ClO_2的爆炸特性，考查了气体ClO_2的爆炸极限及浓度对爆炸压力、爆炸诱导时间的影响。得出了气体ClO_2的爆炸下限为9．5％(体积比)，爆炸上限为100％；气体ClO_2的爆炸压力随浓度的增加而增大，最大爆炸压力出现的诱导时间随着气体ClO_2浓度的增加而缩短。提出了气体ClO_2的爆炸属于分解爆炸，其爆炸机理是涉及到中间稳定物——Cl_2O_3的特殊衰减支链分解爆炸机理，Cl_2O_3是引发、促进支链反应的主要因素。
(4)高纯度气体ClO_2生成系统装置研究
利用安全原理设计了高纯气体ClO_2反应器，ClO_2发生量达到了1．5kg／次以上，NaClO_2转化率达到93．7％、NaClO_3转化率达到95．5％时，气体ClO_2的产率最高达到97．3％，纯度达到了98．55％以上。NaClO_3—NaClO_2组合工艺生成高纯度的气体ClO_2，控制反应时间在30～45min左右较好。理论产量与实际产量二者的偏差在6．2％以内；超出此时间范围，实际产量与动力学计算结果的偏差会越来越大。
(5)气体ClO_2的应用研究
a高纯度气体ClO_2对葡萄的杀菌保鲜研究
研究了气体ClO_2对葡萄表面致病菌——葡萄球菌、大肠杆菌、李斯特单增菌和腐生酵母菌的杀菌效果。得出了气体ClO_2浓度增加和杀菌时间的延长，可以使杀菌效果很快的提高，在气体ClO_2杀菌浓度为25mg/L、杀菌时间12min、杀菌温度25℃的较佳条件下，金黄色葡萄球菌、李斯特单增菌和腐生酵母菌均减少了6．4log量级以上，而大肠杆菌达到5．76log量级。ClO_2的作用浓度和杀菌时间存在协同增效的作用。气体ClO_2对葡萄的保鲜效果研究表明，常温下采用浓度为30ml／m~3的气体ClO_2处理葡萄效果最好。ClO_2可以迅速有效地阻止蛋氨酸的分解，消除乙烯等物质并杀灭腐败菌，从而延缓果蔬变质过程，减少营养成分损失，起到长期保鲜的作用。
b二氧化氯消毒城市生活废水研究
研究表明，污水中粪大肠菌的灭菌效果随着ClO_2浓度和作用时间的增加而增加，得出了ClO_2消毒城市污水的投药浓度为5 mg／L、杀菌时间为20min的最佳条件，粪大肠菌杀菌率达到99．99％的去除率极限。处理后的出水中未检出CHCl_3，CCl_4的含量虽然随ClO_2浓度不同而有所区别，但是含量很少且差别不大。研究结果证实ClO_2消毒水体形成卤代烃类明显低于普通含氯消毒剂，将ClO_2用于污水消毒增强了回用污水的环境安全性。
It is the most effective countermove to exploit the highly active germicidal agentagainst the lethality of biological weapon.ClO_2 gas has attracted attention in the views ofbroad spectrum and highly active bactericidal ability and few or none poisonous byproducts.In this paper,the formative technology of high-purity ClO_2 gas,kinetics of its reaction andbactericidal effect were studied.
(1) Study on the generation of high-purity ClO_2 gas and the determination of itsconcentration and purity
A new technology used the NaClO_3-NaClO_2 compound mode to generated ClO_2 gas wasset forth.The reaction of HCl and NaClO_3 was proceed in main reactor,and,the generatedgaseous mixture containing Cl_2 and ClO_2 enter into the fixed bed reactor loaded NaClO_2granule,where Cl_2 was inverted into ClO_2,and the ClO_2/Cl_2 is 60/1 approximately in the endproducts,the purity of ClO_2 was up to 98.19%.The colorimetric card and test cardcorresponding to concentration of ClO_2 rapid determination were prepared,and the errorpercentage was less than 10% in test specification 5～1000mg/L.
(2) The kinetics of the formation reaction of high-purity ClO_2 gas
The mechanics hypothesis about chemical reaction of HCl and NaClO_3 was set forth,andbeen verified furtherly.The fixed bed and equivalent particle model was established bymicrostructure analysis of gas-solid reaction of NaClO_2 and Cl_2,and the reaction kineticsmodel,using NaClO_3-NaClO_2 compound technology to generate high-purity ClO_2 gas wasobtained.
(3) The explosion characteristics and mechanics of ClO_2 gas
It was the first time for the explosion characteristics of ClO_2 gas was studied in acylindrical exploder with a shell capacity of 20 liters.The impact of concentration toexplosion limit,explosion pressure and induction time were determinated.The experimentalresults indicated that the lower concentration limit for the explosive decomposition ofchlorine dioxide gas was 9.5% ([ClO_2]/[air]),the upper concentration limit was 100%,and thepressure of explosion increased with increasing concentration of ClO_2 gas,the induction time(the time from the moment of sparking to explosion) to attain the maximum pressure of explosion was shorten with increasing concentration of ClO_2 gas.The explosion reaction styleof ClO_2 is decomposition,the reaction mechanism of ClO_2 is of a degenerate chain-branchingtype involving the formation of a stable intermediate Cl_2O_3,and it is the major factor toinitiating and accelerating branched chain reaction.
(4) System device for generating high-purity ClO_2 gas
Following the principle of safety,the reactor to generated high-purity ClO_2 gas wasprepared.The production capacity of ClO_2 gas attained 1.5kg/batch,the percent conversion ofNaClO_2 and NaClO_3 were up to 93.7% and 95.5% respectively,the productive rate of ClO_2gas attained 97.3%,its purity was more than 98.55%.The optimum reaction time range wasfrom 30 to 45 minutes,the deviation of ClO_2 yield between theoretically,and,actually,was nomore than 6.2%,but the deviation of actual output to computing result by dynamics methodbecame more and more when the reaction time exceed the optimum range.
(5) Research on the application of ClO_2 gas
a Effect of ClO_2 gas on bactericidal and keep fresh on grape
The regularity of sterilization to Staphylococcus Aureus,Escherichia Coli 0157.H7,Listeria Monocytogenes and Saprophytic Yeast on grape surface with ClO_2 gas were studiedin this paper.The result showed that the bactericidal effect was markedly increased alongwith the concentration increased of ClO_2 gas and the bactericidal time in the experiment range.When the ClO_2 gas concentration 25mgl~(-1),bactericidal time 12min and temperature 25℃,Staphylococcus Aureus,Listeria Monocytogenes and Saprophytic Yeast decreased more than6.41og,but the decrease of Escherichia Coli 0157:H7 attained 5.761og.There exist synergismeffect between the bactericidal time and ClO_2 concentration.The result also showed that itwas best condition for grape to keep fresh when the concentration of ClO_2 gas is 30ml/m~3,ClO_2 gas can inhibit effectively methionine catabolic process decrease,the generating ofethene when killing the Saprospira on the surface of fruit and vegetable,so it is useful todelay metamorphic process,reduce nutritional ingredient loss,and keep the fruit andvegetable fresh for a long time.
b The municipal wastewater disposal by ClO_2
The result showed that the sterilizing effect to bacillus coli was increasing with theconcentration of ClO_2 and the treating duration increasing,the optimum were ClO_2concentration 5mg/L and bactericidal time 20min,the bactericidal ratio to bacillus coli was99.99%,which is limit bactericidal limit.After wastewater disposal,the CHCl_3 had not been detected in the water,the content of ClC_4 existed difference in some degree with the differentClO_2 concentration,but the real content is lower.The results indicate that the content ofhalogenated hydrocarbon are less than other common chlorine disinfectors after wastewaterare disposed by ClO_2,therefore,environment security is enhanced by using the ClO_2 gas tosterilized recycle-water.
引文
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