基于废物最小的O，S-二甲基硫代磷酰胺连续生产过程开发
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摘要
随着人们对环境与能源关注程度的越来越强烈,近年来从源头上减少污染与进行污染预防控制已成为人们研究的热点,也成为企业可持续发展的必然选择。间歇反应或分批操作过程是精细化工领域的一个常见的生产方式,主要具有简单、灵便、投资少等特点。但是,一般都存在设备效率低、生产能力小、劳动强度大、反应结果易波动以及废物处理难度大等问题。开发连续生产过程具有:更有效的利用能量与原料,回收反应热,强化混合过程以提高选择性降低废物产生,最大限度地减少反应过程的失控,减少工厂的场地和降低工厂的投资,易于实现自动化等特点。提出利用环境影响指标原料利用率(BA)与单位潜在废物产率(MB)对O,S-二甲基硫代磷酰胺及其中间体O-甲基硫代磷酰二氯、O,O-二甲基硫代磷酰氯、O,O-二甲基硫代磷酰胺等连续反应过程进行废物最小化分析,研究上述过程连续生产的实现方式以及相关的理论,对于降低产品的能耗,稳定提高产品的质量与收率,实现清洁化生产,具有十分重要的理论意义与实际应用价值。
以文献报道的O-甲基硫代磷酰二氯合成的动力学为基础,基于废物最小化分析,建立循环管式反应器串联管式反应器连续合成O-甲基硫代磷酰二氯的反应器模型。适当缩短循环管式反应器的停留时间,降低反应温度,可提高O-甲基硫代磷酰二氯的质量与收率。减少甲醇与三氯硫磷的摩尔配比,可有效减少过程的废物产生量。在模拟计算的基础上,建立一套12000吨/年循环管式反应器串联管式反应器连续生产O-甲基硫代磷酰二氯的工业生产装置。工业生产装置连续运行表明:O-甲基硫代磷酰二氯的收率比现有工艺收率提高1.5%,单套装置的生产能力是现有单套装置生产能力的5倍。
在O,O-二甲基硫代磷酰氯合成反应动力学研究的基础上,提出多级循环管式反应器串联连续合成O,O-二甲基硫代磷酰氯的反应器网络。以O,O-二甲基硫代磷酰氯的总收率为优化目标,以MATLAB为编程语言,采用复形法优化等温下各级循环管式反应器内的加碱量。适当增加串联级数、减少循环比、降低反应温度有利于O,O-二甲基硫代磷酰氯收率与产品质量的提高。模拟计算结果表明,6级循环管式反应器串联,在优化的条件下,O,O-二甲基硫代磷酰氯的收率为93.86%,产品摩尔质量达到94.35%。工业单级循环反应器的中试结果与模型计算结果比较吻合,可为工业规模连续生产装置的设计与优化提供理论指导。
研究O,O-二甲基硫代磷酰氯液相非催化氨解的反应动力学。在反应前期,酰氯浓度对速率影响很小,但在反应后期,反应速率呈明显的二级反应特征。氨与酰氯的起始摩尔比以及氨浓度对反应速率影响显著。基于废物最小化分析与反应动力学研究,提出循环管式反应器连续合成O,O-二甲基硫代磷酰胺的绿色过程新工艺,并对循环管式反应器进行模拟与仿真。在模拟计算的基础上,建立一套25000吨/年O,O-二甲基硫代磷酰氯连续氨解的工业生产装置。工业连续生产新工艺的产品质量提高了0.74%,收率提高了2.93%。单套装置生产能力是分批间歇搅拌反应釜单套装置生产能力的7倍,且可大幅度降低产品的能源消耗。
采用单纯形优化法研究O,O-二甲基硫代磷酰胺异构的反应动力学。反应速率对硫酸二甲酯浓度与O,O-二甲基硫代磷酰胺浓度分别为一级反应。对全混釜串联管式反应器连续合成O,S-二甲基硫代磷酰胺的模拟计算标明,采用优化的方案,可使产品收率达到83.7%,比现有间歇生产工艺提高1.2%～1.7%左右。以最大总收率与最大单位潜在废物产率为多目标优化,利用线性加权和法将多目标优化问题转化为单目标优化问题,以MATLAB为编程语言,采用复形法优化反应-分离-再循环(RSR)系统的工艺参数。较低的蒸馏压力有利于提高总收率与提高单位潜在废物的产率。提高O,O-二甲基硫代磷酰胺的质量,可明显提高单位潜在废物的产率。模拟结果表明:采用RSR系统可使产品O,S-二甲基硫代磷酰胺的质量分数达到85%以上,总收率达到96%。在此基础上,提出异构-分子蒸馏分离的绿色集成工艺,具有良好的应用前景。
There is currently a great deal of interest in the development of methods that can be used to prevent or at least minimize the generation of pollution w-ith the people caring about the environment and energy. It has been the neces-sary option for the sustainable development of factory. Batch chemical process is the usual process in producing fine chemical product.It is simple, convenientand small investment in producing many products.But its production capacity issmall, labouring extent is great and it depends on worker’s experience. So the quality and the yield of product is unstable and there is always much waste todeal with.In contrast,the benefits of continuous process include: More efficient utilization of energy and raw materials. Recovery of heats of reaction.High-int-ensity mixing, enhancing process selectivity, minimised risk of runaway reaction,smaller plant, cheaper plant,process automation.The enviroment impact assessme-nt(EIA):efficiency of raw material (BA) and the ratio of product mass to unde-sirable material mass (MB) was proposed to be used to analyse the minimizati-on of waste in the continuous producing O,S-dialkyl phosphoroamidothioate and its intermediate O-miethyl dichlorothiophosphate, O,O-dimethyl phosphorochori-dothioate,O,O-dimethyl phosphoroamidothioate. It has important signifycance th-eoretically and practical application to develop continuous producing process to replace traditional batch chemical process when the production capacity is enl-arged. It can rise the quality and yield of product, decrease the rate of equip-ment size to production capacity, decrease energy consumption, bring about cle-aner production.
The model of continuous producing O-miethyl dichlorothiophosphate reactor was based on the kinetics of synthesizing O-miethyl dichlorothiophosphate which was proposed by previous literature.The retention time of recycle tubular reactor is shorter and the temperature of reaction is lower, the quality and the yield of product is rised.The mole ratio of thiophosphoryl chloride to methanol is decreased ,the waste of the process is reduced.12000 ton/y of recycle reactor series connection tubular reactor was built in a factory.It indicates that the quality and the yield of product is rised about 1.5% and the production capacity of one set equipment is 5 times compared with one set batch reactor.
The reaction kinetics of O,O-dimethylphosphorochloridothioate synthesis wasstudied.Multistage recycle tubular reactors in series was founded to produce O,O-dimethyl phosphorochloridothioate continuously. The amount of alkali was optimized on the objective of the total yield of O,O-dimethylphosphorochlorido-thioate with complex methods optimization by MATLAB.When the stage of ser-ies is increased, the ratio of recycle is reduced, the reaction temperature is do-wn,the quality and the yield of product is rised. The quality can reach 94.35%and the yield can reach above 93.86% in optimal conditions when six stages recycle tubular reactors in series. The pilot-scale experimental result of one re-cycle tubular reactor agrees well with the calculation value by model. It provi-des guide for designing and optimizing the equipment in industrial producing process.
The ammonolysis reaction kinetics of O,O-dimethylphosphorochloridothioate without catalyst was studied. The model showes that the effects of the initial mole ratio between ammonia and acyl chloride, concentration of ammonia and temperature on the reaction rate are very obvious. In addition, the effect of concentration of acyl chloride on the rate of ammonolysis is very small.The reaction rate demonstrates the pseudo-first order to ammonia during early period of reaction and the second order to ammonia and acyl halide during the late period. A new green process is proposed to produce O,O-dialkyl phosphoroamidothioate continuously by recycle tubular reactor with the analysis of waste minimization and the study of reaction kinetics. 25kt/y of recycle tubular reactor was built .It is indicated that the quality and the yield of product is rised 0.74% and 2.93% individually. The production capacity of one set equipment is 7 times compared with batch reactor.It can decrease a great deal of energy consumption.
The isomerization reaction kinetic of O,O-dialkyl phosphoroamidothioate was studied by simplex optimization.The rate of isomerization behaves the firstorder to dimethyl sulphate and O,O-dialkyl phosphoroamidothioate individually.A model of CSTR seried tubular reactor was founded to produce O,S-dimethyl phosphorochloridothioate continuously. It is indicated that the yield of product is rised 1.2%～1.7% in optimal conditions contrast to batch process.A questionof mult-objective optimization was built about reaction-separtion-recycle system.It was optimized to maximize the total yield and the ratio of product mass towaste mass. The mult-objective optimization was converted to simple objective optimization by linear synthesis.The lower distillation pressure can increase the total yield and the ratio of product mass to undesirable material mass. When the quality of O,O-dialkyl phosphoroamidothioate is rised, the ratio of product mass to undesirable material mass can be increased obviously. It indicates that the quality can reach above 85% and the total yield of O,S-dialkyl phosphoro-amidothioate can reach 96%. The green integration flowsheet of isomerization-molecular distillation-recycle is proposed. It has good application foreground in industrial process.
以文献报道的O-甲基硫代磷酰二氯合成的动力学为基础,基于废物最小化分析,建立循环管式反应器串联管式反应器连续合成O-甲基硫代磷酰二氯的反应器模型。适当缩短循环管式反应器的停留时间,降低反应温度,可提高O-甲基硫代磷酰二氯的质量与收率。减少甲醇与三氯硫磷的摩尔配比,可有效减少过程的废物产生量。在模拟计算的基础上,建立一套12000吨/年循环管式反应器串联管式反应器连续生产O-甲基硫代磷酰二氯的工业生产装置。工业生产装置连续运行表明:O-甲基硫代磷酰二氯的收率比现有工艺收率提高1.5%,单套装置的生产能力是现有单套装置生产能力的5倍。
在O,O-二甲基硫代磷酰氯合成反应动力学研究的基础上,提出多级循环管式反应器串联连续合成O,O-二甲基硫代磷酰氯的反应器网络。以O,O-二甲基硫代磷酰氯的总收率为优化目标,以MATLAB为编程语言,采用复形法优化等温下各级循环管式反应器内的加碱量。适当增加串联级数、减少循环比、降低反应温度有利于O,O-二甲基硫代磷酰氯收率与产品质量的提高。模拟计算结果表明,6级循环管式反应器串联,在优化的条件下,O,O-二甲基硫代磷酰氯的收率为93.86%,产品摩尔质量达到94.35%。工业单级循环反应器的中试结果与模型计算结果比较吻合,可为工业规模连续生产装置的设计与优化提供理论指导。
研究O,O-二甲基硫代磷酰氯液相非催化氨解的反应动力学。在反应前期,酰氯浓度对速率影响很小,但在反应后期,反应速率呈明显的二级反应特征。氨与酰氯的起始摩尔比以及氨浓度对反应速率影响显著。基于废物最小化分析与反应动力学研究,提出循环管式反应器连续合成O,O-二甲基硫代磷酰胺的绿色过程新工艺,并对循环管式反应器进行模拟与仿真。在模拟计算的基础上,建立一套25000吨/年O,O-二甲基硫代磷酰氯连续氨解的工业生产装置。工业连续生产新工艺的产品质量提高了0.74%,收率提高了2.93%。单套装置生产能力是分批间歇搅拌反应釜单套装置生产能力的7倍,且可大幅度降低产品的能源消耗。
采用单纯形优化法研究O,O-二甲基硫代磷酰胺异构的反应动力学。反应速率对硫酸二甲酯浓度与O,O-二甲基硫代磷酰胺浓度分别为一级反应。对全混釜串联管式反应器连续合成O,S-二甲基硫代磷酰胺的模拟计算标明,采用优化的方案,可使产品收率达到83.7%,比现有间歇生产工艺提高1.2%～1.7%左右。以最大总收率与最大单位潜在废物产率为多目标优化,利用线性加权和法将多目标优化问题转化为单目标优化问题,以MATLAB为编程语言,采用复形法优化反应-分离-再循环(RSR)系统的工艺参数。较低的蒸馏压力有利于提高总收率与提高单位潜在废物的产率。提高O,O-二甲基硫代磷酰胺的质量,可明显提高单位潜在废物的产率。模拟结果表明:采用RSR系统可使产品O,S-二甲基硫代磷酰胺的质量分数达到85%以上,总收率达到96%。在此基础上,提出异构-分子蒸馏分离的绿色集成工艺,具有良好的应用前景。
There is currently a great deal of interest in the development of methods that can be used to prevent or at least minimize the generation of pollution w-ith the people caring about the environment and energy. It has been the neces-sary option for the sustainable development of factory. Batch chemical process is the usual process in producing fine chemical product.It is simple, convenientand small investment in producing many products.But its production capacity issmall, labouring extent is great and it depends on worker’s experience. So the quality and the yield of product is unstable and there is always much waste todeal with.In contrast,the benefits of continuous process include: More efficient utilization of energy and raw materials. Recovery of heats of reaction.High-int-ensity mixing, enhancing process selectivity, minimised risk of runaway reaction,smaller plant, cheaper plant,process automation.The enviroment impact assessme-nt(EIA):efficiency of raw material (BA) and the ratio of product mass to unde-sirable material mass (MB) was proposed to be used to analyse the minimizati-on of waste in the continuous producing O,S-dialkyl phosphoroamidothioate and its intermediate O-miethyl dichlorothiophosphate, O,O-dimethyl phosphorochori-dothioate,O,O-dimethyl phosphoroamidothioate. It has important signifycance th-eoretically and practical application to develop continuous producing process to replace traditional batch chemical process when the production capacity is enl-arged. It can rise the quality and yield of product, decrease the rate of equip-ment size to production capacity, decrease energy consumption, bring about cle-aner production.
The model of continuous producing O-miethyl dichlorothiophosphate reactor was based on the kinetics of synthesizing O-miethyl dichlorothiophosphate which was proposed by previous literature.The retention time of recycle tubular reactor is shorter and the temperature of reaction is lower, the quality and the yield of product is rised.The mole ratio of thiophosphoryl chloride to methanol is decreased ,the waste of the process is reduced.12000 ton/y of recycle reactor series connection tubular reactor was built in a factory.It indicates that the quality and the yield of product is rised about 1.5% and the production capacity of one set equipment is 5 times compared with one set batch reactor.
The reaction kinetics of O,O-dimethylphosphorochloridothioate synthesis wasstudied.Multistage recycle tubular reactors in series was founded to produce O,O-dimethyl phosphorochloridothioate continuously. The amount of alkali was optimized on the objective of the total yield of O,O-dimethylphosphorochlorido-thioate with complex methods optimization by MATLAB.When the stage of ser-ies is increased, the ratio of recycle is reduced, the reaction temperature is do-wn,the quality and the yield of product is rised. The quality can reach 94.35%and the yield can reach above 93.86% in optimal conditions when six stages recycle tubular reactors in series. The pilot-scale experimental result of one re-cycle tubular reactor agrees well with the calculation value by model. It provi-des guide for designing and optimizing the equipment in industrial producing process.
The ammonolysis reaction kinetics of O,O-dimethylphosphorochloridothioate without catalyst was studied. The model showes that the effects of the initial mole ratio between ammonia and acyl chloride, concentration of ammonia and temperature on the reaction rate are very obvious. In addition, the effect of concentration of acyl chloride on the rate of ammonolysis is very small.The reaction rate demonstrates the pseudo-first order to ammonia during early period of reaction and the second order to ammonia and acyl halide during the late period. A new green process is proposed to produce O,O-dialkyl phosphoroamidothioate continuously by recycle tubular reactor with the analysis of waste minimization and the study of reaction kinetics. 25kt/y of recycle tubular reactor was built .It is indicated that the quality and the yield of product is rised 0.74% and 2.93% individually. The production capacity of one set equipment is 7 times compared with batch reactor.It can decrease a great deal of energy consumption.
The isomerization reaction kinetic of O,O-dialkyl phosphoroamidothioate was studied by simplex optimization.The rate of isomerization behaves the firstorder to dimethyl sulphate and O,O-dialkyl phosphoroamidothioate individually.A model of CSTR seried tubular reactor was founded to produce O,S-dimethyl phosphorochloridothioate continuously. It is indicated that the yield of product is rised 1.2%～1.7% in optimal conditions contrast to batch process.A questionof mult-objective optimization was built about reaction-separtion-recycle system.It was optimized to maximize the total yield and the ratio of product mass towaste mass. The mult-objective optimization was converted to simple objective optimization by linear synthesis.The lower distillation pressure can increase the total yield and the ratio of product mass to undesirable material mass. When the quality of O,O-dialkyl phosphoroamidothioate is rised, the ratio of product mass to undesirable material mass can be increased obviously. It indicates that the quality can reach above 85% and the total yield of O,S-dialkyl phosphoro-amidothioate can reach 96%. The green integration flowsheet of isomerization-molecular distillation-recycle is proposed. It has good application foreground in industrial process.
引文
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