合成聚异戊二烯胶乳制备中蒸馏操作工艺的优化

doi:10.19894/j.issn.1000-0518.250050

摘要/Abstract

摘要：

针对合成聚异戊二烯胶乳制备过程中的关键环节-含溶剂异戊二烯乳液的溶剂脱除工艺，系统考察了蒸馏操作参数对脱溶剂效果的影响。研究重点分析了蒸馏温度、平均停留时间、溶剂脱除率和固含量等关键参数，并对不同蒸馏方式进行了对比实验。结果表明，采用多级串联与并联相结合的连续蒸馏工艺（如一釜三并联再与第四釜串联，且四釜温度不超过78 ℃）一釜最优蒸馏温度在70~72 ℃、平均停留时间在5.5~6.5 h时，溶剂脱除率可达65%~75%，出料固含量（质量分数）约9%，凝胶含量（质量分数）小于2%；在保持工艺参数稳定的条件下，可有效提高蒸馏设备利用率和胶乳处理能力。该研究为工业生产的溶剂脱除工艺优化提供了技术参考。

关键词: 聚异戊二烯胶乳, 生产工艺, 连续法, 并串联

Abstract:

This study systematically investigated the solvent removal process from isoprene emulsion containing solvents， a critical step in synthetic polyisoprene latex production. The research focused on analyzing the effects of continuous distillation parameters， including distillation temperature， average residence time， solvent removal efficiency， and solid content， while comparing different distillation configurations. The results indicated that when the optimal distillation temperature in a single kettle ranged from 70~72 ℃ and the average residence time was between 5.5~6.5 h， the solvent removal rate could reach 65%~75%， with an outlet solid content of approximately 9% and a gel content of less than 2%. By adopting a continuous distillation process that combined multi-stage series and parallel configurations （e.g.， three parallel kettles in series with a fourth kettle， with the temperature in all four kettles not exceeding 78 ℃）， it was possible to effectively enhance the utilization rate of distillation equipment and the processing capacity of latex while maintaining stable process parameters. This study provides technical references for optimizing solvent removal processes in industrial production.

Key words: Polyisoprene latex, Production process, Continuous method, Parallel and tandem

中图分类号:

O631.5

赵洪福, 卜宇轩, 吕小军, 赵卿波, 王红红, 申凯华, 施全宝. 合成聚异戊二烯胶乳制备中蒸馏操作工艺的优化[J]. 应用化学, 2026, 43(2): 249-258.

Hong-Fu ZHAO, Yu-Xuan BU, Xiao-Jun LYU, Qing-Bo ZHAO, Hong-Hong WANG, Kai-Hua SHEN, Quan-Bao SHI. Optimization of Atmospheric Pressure Continuous Distillation Process of Isoprene Latex[J]. Chinese Journal of Applied Chemistry, 2026, 43(2): 249-258.

图/表 19

图1 双釜并联全系统工艺流程图V： Storage tank； S： Agitated vessel/stirred tank； E： Heat exchanger； P： Pump； C： Centrifugal machine

Fig.1 Double kettle parallel connection whole system process flow diagram

表1 间歇法脱除溶剂单元胶乳状况

Table 1 The process of eliminating solvents from polyisoprene latex with batch distillation

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
68~74	12.5	92.7	18.8	Unremovable foam
68~72	14.0	95.5	20.1	Unremovable foam
69~73	13.2	94.6	18.5	Unremovable foam
68~72	12.8	90.8	19.7	Unremovable foam
68~73	13.7	93.7	19.3	Unremovable foam

图2 双釜串联连续蒸馏装置示意图

Fig.2 Sketch of a tandem continuous distillation unit with two vessels

表2 连续化蒸馏脱除溶剂的一级蒸馏釜状况

Table 2 Status of the primary distillation vessel in continuous solvent remova

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
66	8.5~9.0	55~60	0.34	Less foam， evanescent， calm state
67	8.5~9.0	60~65	0.49	Less foam， evanescent， calm state
69	8.5~9.0	75~80	0.46	Less foam， evanescent， calm state
69	7.0~7.5	50~55	0.48	Less foam， evanescent， calm state
70	7.0~7.5	70~75	0.50	More foam， fleeting， calm state
71	7.0~7.5	80~85	0.60	More foam， fleeting， calm state
72	7.0~7.5	90~95	0.60	More foam， fleeting， calm state

图3 蒸馏温度对一级蒸馏釜脱除溶剂的影响A. Feed rate: 3 g/min, average residence time: 8.5~9 h, vessel volume: 2 L, loading coefficient: 75%; B. Feed rate: 4 g/min, average residence time: 7~7.5 h, vessel volume: 2 L, loading coefficient: 75%

Fig.3 Impact of distillation temperature on solvent stripping efficiency in the first-stage distillation vessel

表3 连续化蒸馏脱除溶剂的二级蒸馏釜状况

Table 3 Status of the secondary distillation vessel in continuous solvent remova

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
76	4.0~4.5	15~25	0.92	Less foam， calm state
78	4.0~4.5	25~35	0.90	Foam increases
80	4.0~4.5	-	3.36	A large amount of foam

图4 蒸馏温度对二级蒸馏釜脱除溶剂的影响Feed rate： 6 g/min； Average residence time： 4~4.5 h； Vessel volume： 2 L； Loading coefficient： 75%

Fig.4 Impact of distillation temperature on solvent stripping efficiency in the secondary distillation vessel

表4 平均停留时间对连续化蒸馏脱除溶剂的一级蒸馏釜影响

Table 4 Impact of average residence time on solvent stripping efficiency in the primary continuous distillation vessel

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
71	7.0~7.5	85~90	0.24	Less foam， calm state
71	6.0~6.5	65~70	0.37	Less foam， calm state
71	5.5~6.0	60~65	0.37	Less foam， calm state
74	5.5	70~75	0.49	Foam increases
74	5.0	70	0.50	Foam increases

图5 连续化蒸馏过程一级蒸馏釜溶剂脱除率变化Temperature： 71 ℃； Vessel volume： 2 L； Loading coefficient： 75%

Fig.5 Variation of solvent removal efficiency in the first-stage continuous distillation vessel

表5 平均停留时间对连续化蒸馏脱除溶剂的二级蒸馏釜影响

Table 5 Impact of average residence time on solvent stripping efficiency in the secondary continuous distillation vessel

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
76	8.0	40~45	0.92	Less foam， calm state
76	4.5	15~25	0.68	Less foam， calm state
76	3.0	20~25	0.98	Less foam， calm state
78	4.5	25~30	0.90	Foam increases
78	3.0	25~35	0.95	Foam increases
78	2.5	30~40	2.24	A large amount of foam

图6 连续化蒸馏过程一级蒸馏釜溶剂脱除率变化A. Temperature: 76 ℃, vessel volume: 2 L, loading coefficient: 75%; B. Temperature: 78 ℃, vessel volume: 2 L， loading coefficient: 75%

Fig.6 Variation of solvent removal efficiency in the secondary continuous distillation vessel

图7 两釜并联加串联连续蒸馏装置示意图

Fig.7 Sketch of parallel connection with series configuration of two distillation vessels

图8 双釜串联加串联单釜连续化蒸馏过程中二级蒸馏釜平衡过程Feed rate： 6 g/min； Average residence time： 4 ~ 4.5 h； Vessel volume： 2 L； Loading coefficient： 75%

Fig.8 Fluctuation of solvent stripping rate of stage-2 vessel in twin-series continuous distillation system

图9 三釜并联加串联连续蒸馏装置示意图

Fig.9 Sketch of parallel connection with series configuration of three distillation vessels

图10 三釜串联加串联单釜连续化蒸馏过程中二级蒸馏釜平衡过程Feed rate： 9 g/min； Average residence time： 3.0 h； Vessel volume： 2 L； Loading coefficient： 75%

Fig.10 Fluctuation of solvent stripping rate of stage-2 vessel in three-series continuous distillation system

图11 四釜并联加串联连续蒸馏装置示意图

Fig.11 Sketch of parallel connection with series configuration of four-unit distillation vessels

表6 双釜串联加串联单釜连续化蒸馏过程中二级蒸馏釜状况

Table 6 Performance of stage-2 vessel in twin-series continuous distillation system

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
76	4.2~4.5	15~25	0.68	Less foam， calm state
78	4.2~4.5	25~30	0.90	Foam increases

表7 三釜串联加串联单釜连续化蒸馏过程中二级蒸馏釜状况

Table 7 Performance of stage-2 vessel in three-series continuous distillation syste

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
76	3	15~25	0.98	Less foam， calm state
78	3	25~30	0.95	Foam increases

表8 四釜串联加串联单釜连续化蒸馏过程中二级蒸馏釜状况

Table 8 Performance of stage-2 vessel in four-series continuous distillation syste

Distillation temperature/℃	Distillation duration/h	Solvent removal rate/%	Gel loss/%	Phenomenon
78	2.5	35~45	2.24	A large amount of foam
80	2.5	25~35	3.36	A large amount of foam

参考文献 9

[1]	赵瑞，刘琼玲，樊翌明. 医护人员乳胶手套过敏的研究进展［J］. 中华护理教育， 2014， 11（3）： 223-225.
	ZHAO R， LIU Q L， FAN L M. Research progress on latex glove allergy among healthcare workers［J］. Chin J Nurs Educ， 2014， 11（3）： 223-225.
[2]	吕小军，赵卿波，赵洪福，等. 用稀土聚异戊二烯橡胶制备人造异戊胶乳的乳化体系及制备工艺［J］. 合成橡胶工业， 2025， 48（2）： 92-96.
	LV X J， ZHAO Q B， ZHAO H F， et a1. Emulsification system and preparation process of artificial isoprene rubber latex using rare earth polyisoprene rubber［J］. China Synth Rubber Ind， 2025， 48（2）： 92-96.
[3]	朱永康. Cariflex公司计划在新加坡建设世界最大聚异戊二烯胶乳工厂［J］. 橡胶科技， 2022， 20（12）： 618.
	ZHU Y K. Cariflex Company plans to build the world's largest polyisoprene latex factory in Singapore［J］. Rubber Sci Technol， 2022， 20（12）： 618.
[4]	王红红. 人造聚异戊二烯胶乳连续化工艺的调控研究［D］. 大连：大连理工大学， 2024.
	WANG H H. Study on the controllable preparation of artificial latex with polyisoprene rubber［D］. Dalian： Dalian University of Technology， 2024.
[5]	MIRI S， POURPAK Z， ZARINARA A， et a1. Prevalence of type I allergy to natural rubber latex and type IV allergy to latex and rubber additives in operating room staff with glove-related symptoms［J］. Allergy Asthma Proc， 2007， 28（5）： 557-563.
[6]	LEUNG R， HO A， CHAN J， et a1. Prevalence of latex allergy in hospital staff in Hong Kong［J］. Clin Exp Allerg， 1997， 27（2）： 167-174.
[7]	A·W·范德瓦尔， M·松德尔曼， S·W·伯恩，等. 科腾聚合物美国有限公司. 人造胶乳的制备办法：中国， 200980126521.9［P］， 2014-03-16.
	VAN DER WAALS A W， SONDERMAN M， BOURNE S W， et al. Kraton Polymers USA， Inc. The method for preparing artificial latex： CN， 200980126521.9［P］， 2014-03-16.
[8]	裴素明，陶俊，池水媛，等. 聚异戊二烯胶乳及其应用现状［J］. 合成橡胶工业， 2014， 37（2）： 150-153.
	PEI S M， TAO J， CHI S Y， et al. Polyisoprene latex and its application status［J］. China Synth Rubber Ind， 2014， 37（2）： 150-153.
[9]	李俊杰. 聚异戊二烯橡胶制备异戊胶乳的工艺研究［D］. 大连：大连理工大学， 2018.
	LI J J. Technical study on the preparation of IRL by IR［D］. Dalian： Dalian University of Technology， 2018.