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HH-CEC 氯代碳酸乙烯酯的合成产物分析专用毛细管柱
2022-07-25 10:40  点击:338
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 氯代碳酸乙烯酯的合成产物分析专用毛细管柱
氯代碳酸乙烯酯的合成产物分析专用毛细管柱 详细信息：

名称：毛细管柱

规格：30m*0.32mm

型号：HH-CEC



采用新型引发剂的氯代碳酸乙烯酯的制备方法,包括以下步骤:1)以碳酸乙烯酯和氯气为反应原料,控制釜温在80～90℃,采用过氧化苯甲酰和邻苯二甲酸二环已酯的混合物作为新型引发剂,并在新型引发剂的作用下反应生成氯代碳酸乙烯酯;2)氯化反应产生的氯化氢和氯气尾气分别用清水和碱液吸收生成副产品含量大于30%浓盐酸和含量大于10%的次氯酸钠;3)将氯代碳酸乙烯酯混合液用转料泵转移脱酸釜中进行脱酸处理,控制脱酸釜温度为90～105℃,边搅拌边抽真空,脱酸5个小时,即可得到水分和酸度较低的氯代碳酸乙烯酯.提供的制备方法能够减少水分带入,缩短反应时间,提高回收效率,适合企业大规模生产.


浩瀚色谱（山东）应用技术开发有限公司，，，研发生产氯代碳酸乙烯酯制备过程测定的专用气相色谱GC-，测定了一氯代碳酸乙烯酯和二氯代碳酸乙烯酯及残存的原料碳酸乙烯酯的含量，柱效高，分离好，峰型对称.此项技术为浩瀚色谱的。
其中原料碳酸乙烯酯（EC）:5.7062%;二氯碳酸乙烯酯（DCEC）:9.46%;氯代碳酸乙烯酯（CEC）:81.14%.



氯代碳酸乙烯酯的合成产物分析专用毛细管柱  测试谱图：




序号

 保留时间

 组分名称

 浓度

 峰面积

 峰高

 结果判定

1

0.979

 

0.0213

1290

293

 

2

1.148

 

0.0859

5194

3981

 

3

1.619

 

0.0411

2485

413

 

4

1.739

 

0.1764

10669

1124

 

5

2.099

 

0.0235

1420

152

 

6

2.549

 

0.0486

2942

189

 

7

3.259

 

0.0265

1601

184

 

8

5.154

 

0.0215

1298

378

 

9

6.224

 

0.0272

1646

552

 

10

7.355

 

0.0229

1388

237

 

11

8.468

 

0.4619

27945

9114

 

12

10.482

 

0.0287

1735

447

 

13

11.267

EC

5.7062

345214

104380

碳酸乙烯酯

14

11.972

 

0.0302

1824

318

 

15

12.584

 

0.2179

13181

3644

 

16

13.119

 

0.0911

5514

1547

 

17

13.470

 

0.0463

2801

746

 

18

13.839

 

0.3849

23287

6486

 

19

14.117

 

0.3071

18582

2902

 

20

14.364

 

0.0282

1708

384

 

21

15.038

DCEC

9.4644

572580

64020

二氯碳酸乙烯酯

22

15.226

 

0.1868

11300

2977

 

23

15.608

 

0.0392

2372

532

 

24

16.297

CEC

81.1464

4909204

399048

氯代碳酸乙烯酯

25

16.813

 

0.0230

1392

296

 

26

17.067

 

0.0382

2312

678

 

27

17.373

 

0.2833

17142

3597

 

28

17.702

 

0.0406

2458

746

 

29

18.118

 

0.0692

4187

1158

 

30

18.573

 

0.1265

7654

1376

 

31

20.102

 

0.0313

1896

446

 

32

20.438

 

0.0197

1190

342

 

33

21.371

 

0.0052

318

160

 

34

21.825

 

0.1062

6426

690

 

35

22.209

 

0.0109

659

319

 

36

22.360

 

0.0202

1223

403

 

37

22.805

 

0.0831

5029

239

 

38

23.450

 

0.1838

11120

911

 

39

23.696

 

0.0346

2091

308

 

40

24.329

 

0.0436

2637

252

 

41

24.570

 

0.0167

1011

277

 

42

24.730

 

0.0101

614

227

 

43

24.917

 

0.0357

2161

236

 

44

25.637

 

0.1837

11112

377

 

  


Special capillary column for analysis of synthetic products of chloroethylene carbonate
Capillary column for the analysis of synthetic products of chloroethylene carbonate Details:

Name: capillary column

Specifications: 30m*0.32mm

Model: HH-CEC



The preparation method of chlorinated ethylene carbonate using a novel initiator comprises the following steps: 1) using ethylene carbonate and chlorine as reaction raw materials, controlling the temperature of the kettle at 80-90 ° C, using benzoyl peroxide and phthalic acid The mixture of dicyclohexyl ester is used as a new type of initiator, and reacts under the action of the new type of initiator to generate chlorinated ethylene carbonate; 2) The hydrogen chloride and chlorine tail gas produced by the chlorination reaction are absorbed with water and lye, respectively, and the content of by-products is greater than 30% % concentrated hydrochloric acid and sodium hypochlorite with a content greater than 10%; 3) transfer the chloroethylene carbonate mixed solution to the deacidification kettle for deacidification treatment with a transfer pump, and control the temperature of the deacidification kettle to be 90 to 105° C. After vacuuming and deacidification for 5 hours, chloroethylene carbonate with low moisture and acidity can be obtained. The provided preparation method can reduce the introduction of moisture, shorten the reaction time, and improve the recovery efficiency, which is suitable for large-scale production of enterprises.


Haohan Chromatography (Shandong) Application Technology Development Co., Ltd., keeping pace with the times and guided by the scientific development concept, has developed and produced a special gas chromatography GC- for the determination of the preparation process of chloroethylene carbonate. The content of dichloroethylene carbonate and the remaining raw material ethylene carbonate, high column efficiency, good separation, and symmetrical peak shape. This technology is unique in the vast chromatography.
Among them, the raw material ethylene carbonate (EC): 5.7062%; dichloroethylene carbonate (DCEC): 9.46%; chloroethylene carbonate (CEC): 81.14%.



Special capillary column for the analysis of synthetic products of chloroethylene carbonate Test chromatogram:

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