CN106596830B - 工业生产中2,4-二氨基甲苯浓度快速检测法 - Google Patents

工业生产中2,4-二氨基甲苯浓度快速检测法 Download PDF

Info

Publication number
CN106596830B
CN106596830B CN201710029409.XA CN201710029409A CN106596830B CN 106596830 B CN106596830 B CN 106596830B CN 201710029409 A CN201710029409 A CN 201710029409A CN 106596830 B CN106596830 B CN 106596830B
Authority
CN
China
Prior art keywords
sample
silica gel
gel plate
concentration
samples
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201710029409.XA
Other languages
English (en)
Other versions
CN106596830A (zh
Inventor
苏德水
邵方
朱建华
黄津
刘月娥
孟凡伟
赵立宁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Antai Fengyuan Environmental Protection Technology Inner Mongolia Group Co ltd
Original Assignee
Hebei Fengyuan Green Technology Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hebei Fengyuan Green Technology Inc filed Critical Hebei Fengyuan Green Technology Inc
Priority to CN201710029409.XA priority Critical patent/CN106596830B/zh
Publication of CN106596830A publication Critical patent/CN106596830A/zh
Application granted granted Critical
Publication of CN106596830B publication Critical patent/CN106596830B/zh
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

本发明公开了一种工业生产中2,4‑二氨基甲苯浓度快速检测法。包括以下步骤：(1)硅胶板的活化和标样的配制；(2)选取具有代表性的样品；(3)对样品进行预处理；(4)检测样品中的浓度值。本发明的优点在于，实现了2,4‑TDA浓度的快速检测，能够达到在生产过程中监测反应程度，控制反应进程的目的，且检测费用低并能满足生产要求。

Description

工业生产中2,4-二氨基甲苯浓度快速检测法
技术领域
本发明涉及薄层色谱法在工业生产中反应液浓度方面的快速测定技术。
背景技术
TDI(甲苯二异氰酸酯)是聚氨酯塑料的主要原料之一，广泛应用于软泡、弹性体、合成革浆料、胶粘合剂、涂料、纤维和皮革织物涂饰剂等生产领域，为高附加值化工产品。但是，工厂在TDI生产过程中，都会产生约占总产量10％的固体废渣。该渣属于危险废物，需要用焚烧的方法才能使其无害化，但同时放出了大量的碳氧化合物、氮氧化合物和烟雾，对环境的负担非常大。为了能够有效回收资源，减小环境负担，河北丰源环保科技股份有限公司通过自主研发，采用水解的方法将TDI废渣在催化剂作用下与水反应生成可回收利用的TDA(甲苯二胺)单体，达到废物资源化利用的目的；经过后续分离提纯，使回收的TDA产品(TDA纯度达98.5％以上)回用于TDI生产过程，真正实现废物利用，循环经济。
该渣的水解过程为一缓慢进程，需在反应过程中对水解的程度进行监控，故此，借助薄层色谱法快速对反应液的浓度进行测定。
发明内容
本发明公开了一种检测方法，用于快速检测工业生产过程中反应液中的2,4-TDA浓度。
本发明的目的由如下技术方案实施：工业生产中2,4-二氨基甲苯浓度快速检测法，其包括以下步骤：(1)硅胶板的活化和标样的配制；(2)选取具有代表性的样品；(3)对样品进行预处理；(4)检测样品中的浓度值。
所述步骤(1)硅胶板的活化温度100℃，活化时间60min；2,4-TDA标准样的浓度为1mg/g，2mg/g，3mg/g，4mg/g，5mg/g，6mg/g，7mg/g，8mg/g，9mg/g，共9个样品，其中溶剂与所要检测的反应液中的溶剂相同。
所述步骤(2)选取具有代表性的样品：用取样管从反应釜取样口进行收集，取带有温度段的样品10ml。
所述步骤(3)对样品进行预处理：摇晃步骤(2)中所取样品使其均匀，用吸管吸取一定量样品并称重，用指定溶剂稀释至所需倍数，摇匀待测。
所述步骤(4)检测样品中的浓度值：用毛细管吸取标液3mm点样于硅胶板上，一般为圆点，点样基线距离底边约1.5cm，点样直径为2-4mm，点间距离约1.0-1.5cm，点间距离可视斑点扩散情况以不影响检出为宜。同样方法，用同一根毛细管吸取待测液3mm点样于硅胶板上，点样时必须注意勿损伤硅胶层表面。用电吹风吹干，约3min。展开室预先用展开剂饱和，在室中加入足够量的展开剂，将点好样品的硅胶板放入展开室的展开剂中，浸入展开剂的深度为距硅胶板底边0.5-1.0cm，密封室盖，等展开距上边界1-1.5cm，取出硅胶板，吹干。把吹干的硅胶板放入碘缸染色2min，取出进行染色点大小的比较，得出样品的浓度值。
优选情况下，所述步骤(2)中指定溶剂为正庚醇、二甘醇、乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、己二醇或其组合。
优选情况下，所述步骤(4)中毛细管内径为0.2-0.4mm。
优选情况下，所述步骤(4)中展开剂为分析纯的石油醚与丙酮以3:8体积比混合溶液。
本发明的优点在于，实现了2,4-TDA浓度的快速检测，能够达到在生产过程中监测反应程度，控制反应进程的目的，且检测费用很低并能满足生产要求。
具体实施方式：
实施例：工业生产中2,4-二氨基甲苯浓度快速检测法(TLC检测法)，其包括以下步骤：(1)硅胶板的活化和标样的配制；(2)选取具有代表性的样品；(3)对样品进行预理；(4)检测样品中的浓度值。
(1)硅胶板在温度100±1℃下活化时间60min。标准样品的配制：用分析天平称取2,4-TDA，配制成浓度为1mg/g，2mg/g，3mg/g，4mg/g，5mg/g，6mg/g，7mg/g，8mg/g，9mg/g，共9个样品的相应溶液。
(2)选取具有代表性的样品：取样过程中，先打开取样阀让反应液流出，待反应液有温度后用玻璃烧杯进行取样，稍凉后摇匀取10ml置于直管中。
(3)对样品进行预处理：取一干净直管，置于分析天平上，置零；用吸管吸取0.2000-0.3000g样品，置于直管中，再用正庚醇稀释至所需倍数。
(4)检测样品中的浓度值：用毛细管吸取4mg/g，5mg/g，6mg/g标液各3mm点样于硅胶板上，点样基线距离底边约1.5cm，点样直径为2-4mm，取点间距离约1.0-1.5cm，再以同样方法将样品点置于同一硅胶板上。用电吹风将全部点吹干。将该硅胶板放入预先放有展开剂的展开室中，浸入展开剂的深度为距硅胶板底边0.5-1.0cm，密封室盖，等展开距上边界1-1.5cm，取出硅胶板，用电吹风吹干。把吹干的硅胶板放入碘缸染色2min，取出硅胶板，比对样品点和标样染色点的大小，得出样品的浓度值。如稀释10倍，样品点和4mg/g的点的大小一致，则浓度为40mg/g，即4％。
结论：该方法通过在生产实践中的应用，已证明其检测结果可以做到快速准确，可以满足工业生产的需要。

Claims (2)

1.一种工业生产中2,4-二氨基甲苯浓度快速检测法，其特征在于，其包括如下检测步骤：
(1)硅胶板的活化和标样的配制；
(2)选取具有代表性的样品；
(3)对样品进行预处理；
(4)检测样品中的浓度值；
所述步骤(1)硅胶板的活化温度100℃，活化时间60min；配制2,4-TDA标准样的浓度为1mg/g，2mg/g，3mg/g，4mg/g，5mg/g，6mg/g，7mg/g，8mg/g，9mg/g，共9个样品；
所述步骤(2)选取具有代表性的样品：用取样管从反应釜取样口进行收集，取带有温度段的样品10ml；
所述步骤(3)对样品进行预处理：摇晃步骤(2)中所取样品使其均匀，用吸管吸取一定量样品并称重，用指定溶剂稀释至所需倍数，摇匀待测；
所述步骤(4)检测样品中的浓度值：用毛细管吸取标液3mm点样于硅胶板上，点样基线距离底边1.5cm，点样直径为2-4mm，点间距离1.0-1.5cm，点间距离可视斑点扩散情况以不影响检出为宜；同样方法，用同一根毛细管吸取待测液3mm点样于硅胶板上；用电吹风吹干；展开室预先用展开剂饱和，在室中加入足够量的展开剂，将点好样品的硅胶板放入展开室的展开剂中，浸入展开剂的深度为距硅胶板底边0.5-1.0cm，密封室盖，等展开距上边界1-1.5cm，取出硅胶板，吹干；把吹干的硅胶板放入碘缸染色2min，取出进行染色点大小的比较，得出样品的浓度值；
所述步骤(4)中展开剂为分析纯的石油醚与丙酮以3:8体积比混合溶液；
所述步骤(4)中毛细管内径为0.2-0.4mm。
2.根据权利要求1所述的工业生产中2,4-二氨基甲苯浓度快速检测法，其特征在于，所述步骤(3)中指定溶剂为正庚醇、二甘醇、乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、己二醇中的一种或多种。
CN201710029409.XA 2017-01-16 2017-01-16 工业生产中2,4-二氨基甲苯浓度快速检测法 Expired - Fee Related CN106596830B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710029409.XA CN106596830B (zh) 2017-01-16 2017-01-16 工业生产中2,4-二氨基甲苯浓度快速检测法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710029409.XA CN106596830B (zh) 2017-01-16 2017-01-16 工业生产中2,4-二氨基甲苯浓度快速检测法

Publications (2)

Publication Number Publication Date
CN106596830A CN106596830A (zh) 2017-04-26
CN106596830B true CN106596830B (zh) 2018-09-28

Family

ID=58584767

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710029409.XA Expired - Fee Related CN106596830B (zh) 2017-01-16 2017-01-16 工业生产中2,4-二氨基甲苯浓度快速检测法

Country Status (1)

Country Link
CN (1) CN106596830B (zh)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6342503B1 (en) * 1993-10-12 2002-01-29 Dupont Pharmaceuticals Company 1N-alkyl-n-arylpyrimidinamines and derivatives thereof
CN102093150A (zh) * 2011-01-07 2011-06-15 北京理工大学 一种合成芳香胺的方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6342503B1 (en) * 1993-10-12 2002-01-29 Dupont Pharmaceuticals Company 1N-alkyl-n-arylpyrimidinamines and derivatives thereof
CN102093150A (zh) * 2011-01-07 2011-06-15 北京理工大学 一种合成芳香胺的方法

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
Determination of 2,4- and 2,6-diaminotoluene in flexible urethane foams;J.L. Guthrle等;《Analytical Chemistry》;19771031;第49卷(第12期);第1676～1680页 *
IDENTIFICATION OF PRIMARY AROMATIC AMINES IN UTAGENICALLY ACTIVE SUBFRACTIONS FROM COALLIQUEFACTION MATERIALS;BARY W. WILSON等;《Mutation Research》;19801231;第79卷;第196页第1-19行 *
染色纺织品上禁用偶氮染料薄层色谱法测定的研究;钱毅等;《现代商检科技》;19961231;第6卷(第5期);第二节，第四节中第1小节、第2小节，表1 *
纺织品禁用偶氮染料薄层色谱法分析方法;秦书琴等;《印染》;19970331;第23卷(第3期);第25～30页 *
钱毅等.染色纺织品上禁用偶氮染料薄层色谱法测定的研究.《现代商检科技》.1996,第6卷(第5期),第1～4页. *

Also Published As

Publication number Publication date
CN106596830A (zh) 2017-04-26

Similar Documents

Publication Publication Date Title
Tobiszewski et al. Green analytical chemistry in sample preparation for determination of trace organic pollutants
St-Pierre et al. Effect of selected airborne contaminants on PEMFC performance
Zhan et al. Highly selective stir bar coated with dummy molecularly imprinted polymers for trace analysis of bisphenol A in milk
CN112763292B (zh) 一种铁素体马氏体双相钢的显微组织显示方法
JP6773138B2 (ja) 分析システム、分析方法及び分析制御プログラム
CN102998463A (zh) 一种测量糖化血红蛋白的方法及试剂盒
CN108828100B (zh) 一种纺织品及皮革制品中硝基苯类化合物的测试方法
RU2012107990A (ru) Способ подготовки образцов для анализа и картридж для него
CN113134400A (zh) 一种可去除气泡的微流控芯片
Chamieh et al. Preparation and full characterization of a micro-immunoaffinity monolithic column and its in-line coupling with capillary zone electrophoresis with Ochratoxin A as model solute
Hu et al. Investigation of ractopamine‐imprinted polymer for dispersive solid‐phase extraction of trace β‐agonists in pig tissues
CN102372821A (zh) 一种邻苯二甲酸二丁酯分子印迹聚合物及其制备方法
CN103833885A (zh) 一种离子液体聚合物毛细管微萃取整体柱及其制备方法
Yuan et al. Sensitive determination of rose bengal in brown sugar by a molecularly imprinted solid-phase extraction monolithic capillary column coupled with capillary electrophoresis
Zhang et al. Preparation of 17β‐estradiol surface molecularly imprinted polymers and their application to the analysis of biological samples
López et al. Characterization of MIPA and DIPA aqueous solutions in relation to absorption, speciation and degradation
CN106596830A (zh) 工业生产中2,4‑二氨基甲苯浓度快速检测法
CN101526490B (zh) 基于可逆固定化酶的量热式生物传感器
CN102134808A (zh) 一种经过拒水处理的纺织品及其生产方法
Lin et al. On-chip sample pretreatment using a porous polymer monolithic column for solid-phase microextraction and chemiluminescence determination of catechins in green tea
Chen et al. Application of an ampholine‐functionalized hybrid organic–inorganic silica material for the SPE of aromatic amines
CN211179858U (zh) 一种血清淀粉样蛋白a层析检测卡
CN113877239A (zh) 一种集成纺织品超声提取及检测的微流控芯片
Stahl et al. High‐Pressure Treatment of Wood–Combination of Mechanical and Thermal Drying in the “I/D Process”
CN206020157U (zh) 一种气体净化装置

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20170426

Assignee: Yuansheng branch of Cangzhou Dahua TDI Co.,Ltd.

Assignor: HEBEI FENGYUAN GREEN TECHNOLOGY Inc.

Contract record no.: X2021980002216

Denomination of invention: Rapid determination of 2,4-Diaminotoluene in industrial production

Granted publication date: 20180928

License type: Common License

Record date: 20210329

EE01 Entry into force of recordation of patent licensing contract
CP03 Change of name, title or address

Address after: 061000 Floor 5, R&D Building, No. 9, Guofeng Avenue, High tech Zone, Cangzhou City, Hebei Province

Patentee after: Hebei Fengyuan Environmental Protection Technology Group Co.,Ltd.

Address before: 061000 south of No.1 Road, Zhongjie Industrial Park, Cangzhou City, Hebei Province

Patentee before: HEBEI FENGYUAN GREEN TECHNOLOGY Inc.

CP03 Change of name, title or address
CP03 Change of name, title or address

Address after: 010000 West Wanda Sales Center, Genghis Khan West Street, Huimin District, Hohhot City, Inner Mongolia Autonomous Region

Patentee after: Antai Fengyuan Environmental Protection Technology (Inner Mongolia) Group Co.,Ltd.

Country or region after: China

Address before: 061000 Floor 5, R&D Building, No. 9, Guofeng Avenue, High tech Zone, Cangzhou City, Hebei Province

Patentee before: Hebei Fengyuan Environmental Protection Technology Group Co.,Ltd.

Country or region before: China

CP03 Change of name, title or address
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Rapid detection method for 2,4-diaminotoluene concentration in industrial production

Granted publication date: 20180928

Pledgee: Baotou Branch of Inner Mongolia Hohhot Jingu Rural Commercial Bank Co.,Ltd.

Pledgor: Antai Fengyuan Environmental Protection Technology (Inner Mongolia) Group Co.,Ltd.

Registration number: Y2024150000015

PE01 Entry into force of the registration of the contract for pledge of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180928

CF01 Termination of patent right due to non-payment of annual fee