CN106554451A - 一种白球生产工艺 - Google Patents

一种白球生产工艺 Download PDF

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CN106554451A
CN106554451A CN201610484686.5A CN201610484686A CN106554451A CN 106554451 A CN106554451 A CN 106554451A CN 201610484686 A CN201610484686 A CN 201610484686A CN 106554451 A CN106554451 A CN 106554451A
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archon
monomer
polymerisation
suspension polymerisation
suspension
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胡天忠
裴红霞
张晓磊
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Ningxia Haicheng Electronic Mdt Infotech Ltd
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Ningxia Haicheng Electronic Mdt Infotech Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/16—Organic material
    • B01J39/18—Macromolecular compounds
    • B01J39/20—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/12—Macromolecular compounds
    • B01J41/14—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/18—Introducing halogen atoms or halogen-containing groups
    • C08F8/24—Haloalkylation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
    • C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/34—Introducing sulfur atoms or sulfur-containing groups
    • C08F8/36—Sulfonation; Sulfation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02—Homopolymers or copolymers of hydrocarbons
    • C08J2325/04—Homopolymers or copolymers of styrene
    • C08J2325/08—Copolymers of styrene

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

本发明涉及化工产品生产领域，尤其是白球生产领域。目前白球的生产工艺主要有喷射聚合和悬浮聚合。悬浮聚合是指溶有引发剂的单体，借助悬浮剂的悬浮作用和机械搅拌，使单体以小液滴的形式分散在介质水中的聚合过程。溶有引发剂的一个单体小液滴，就相当于本体聚合的一个小单元，因此，悬浮聚合也称为本体聚合。悬浮聚合中的主要组分是单体、引发剂、悬浮剂介质（水）。悬浮聚合可根据单体对聚合物溶解与否，将其分为均相悬浮聚合和非均相悬浮聚合。此工艺加工成的白球粒径分布较宽，大小不一，最后必须经振动筛按一定的标准筛分后才能包装入库。它的优点是：生产工艺成熟，生产环节用时短，产品收率高，废水、废气排放量小。聚合物易分离、干燥，后处理简单。

Description

一种白球生产工艺
技术领域
本发明涉及化工产品生产领域，尤其是白球生产领域。
背景技术
目前白球的生产工艺主要有喷射聚合和悬浮聚合。悬浮聚合是指溶有引发剂的单体，借助悬浮剂的悬浮作用和机械搅拌，使单体以小液滴的形式分散在介质水中的聚合过程。溶有引发剂的一个单体小液滴，就相当于本体聚合的一个小单元，因此，悬浮聚合也称为本体聚合。悬浮聚合中的主要组分是单体、引发剂、悬浮剂介质（水）。悬浮聚合可根据单体对聚合物溶解与否，将其分为均相悬浮聚合和非均相悬浮聚合。此工艺加工成的白球粒径分布较宽，大小不一，最后必须经振动筛按一定的标准筛分后才能包装入库。它的优点是：生产工艺成熟，生产环节用时短，产品收率高，废水、废气排放量小。聚合物易分离、干燥，后处理简单。喷射分散聚合就是采用特殊的白球生产设备，喷射单体流在激振下断裂成均匀油滴，油滴进入含有分散稳定剂的介质（水），受热定型，靠浮力上升，泵入熟化罐，进一步固化成型。该工艺不再使用搅拌，所得的白球粒径范围较小，提高了合格范围白球的比例。但因为振动控制和水相流动控制不稳定，避免不了白球聚并，常常出现粒径相同的白球粘连在一起，水相中使用大量的分散稳定剂和高比重的无机盐，使得污水很难处理，也无法避免抽提过程中造成的污染。虽然这种方法使单体微粒的均一率增加了，但是由于生产技术不够成熟，抽取的微粒直径分布还是不理想，以致大部分聚合物不符合要求。另外这是一个连续的生产过程，微粒形成会很慢。这种工艺对于生产离子交换树脂产品所必须的高质量的白球不是很理想。
发明内容
白球生产工艺
在离子交换树脂的生产中小白球是由苯乙烯和二乙烯苯两种单体在过氧化苯甲酰的引发作用下，在去离子水中经适当的搅拌使单体分散成大小合适的液珠，悬浮交联共聚聚合成粒度均匀圆形球体，即白球。它具有特殊的三维网状结构, 聚苯乙烯形成链状高分子,二乙烯苯作为交联剂, 在聚合链之间起搭桥作用。聚苯乙烯-二乙烯苯型共聚物为聚苯乙烯-二乙烯苯型离子交换树脂的高分子骨架，经磺化可制得苯乙烯系强酸性阳离子交换树脂，经氯甲基化反应和胺化反应, 即可制得苯乙烯系季铵型强碱性阴离子交换树脂。
（1）聚合
首先将符合标准的苯乙烯和二乙烯苯称量好，用泵泵入高位槽，放入母液槽中，然后将去离子水加入到反应釜中，随后用真空泵将备好的苯乙烯和二乙烯苯打入反应釜，开启搅拌，自常温逐步升温80-90℃进行聚合反应。聚合过程中取样到放次甲基蓝的表面皿中观察颗粒状况，然后调整搅拌速度，控制颗粒大小。待白球粒度均匀、稳定后，自高位槽放入事先准备好的定量的聚乙烯醇水溶液，继续搅拌30分钟左右，停止搅拌降温。苯乙烯的转化率为99.9%。
当温度降到60℃左右时，液相经反应釜中过滤系统过滤后，排入母液槽中，回收致孔剂后母液供下次使用。
（2）水煮(硬化)
聚合得到的球体硬度较低需要将球体硬化。工艺如下：液相分离后，将固相放入下层水煮釜中，加入自来水，通过夹套加热升温至80-100℃搅拌水煮聚合球体，维持反应1-2小时，使珠体硬化（熟化）。反应结束后，停止加温。待温度降到60℃左右时，经离心机分离固液两相，液相输入液槽中一部分供下次水煮使用，一部分排放。
（3）干燥
将得到的白球通过吊装设备移至真空干燥机中烘干，筛分装袋贮存。白球产品收率为99.45%。
白球反应式为：

Claims (2)

1.本发明涉及原料成分及配比。
2.本发明涉及生产流程：（1）聚合；（2）水煮(硬化)；（3）干燥。
CN201610484686.5A 2016-06-29 2016-06-29 一种白球生产工艺 Pending CN106554451A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110511309A (zh) * 2019-09-06 2019-11-29 无锡迈科为生物科技有限公司 一种磁性高分子微球的制备方法

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JPH072909A (ja) * 1993-02-26 1995-01-06 Mitsubishi Chem Corp 球状架橋共重合体の製造法
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JPH072909A (ja) * 1993-02-26 1995-01-06 Mitsubishi Chem Corp 球状架橋共重合体の製造法
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110511309A (zh) * 2019-09-06 2019-11-29 无锡迈科为生物科技有限公司 一种磁性高分子微球的制备方法

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