CN101786946B - 甲缩醛的制备装置 - Google Patents

甲缩醛的制备装置 Download PDF

Info

Publication number
CN101786946B
CN101786946B CN2010101459420A CN201010145942A CN101786946B CN 101786946 B CN101786946 B CN 101786946B CN 2010101459420 A CN2010101459420 A CN 2010101459420A CN 201010145942 A CN201010145942 A CN 201010145942A CN 101786946 B CN101786946 B CN 101786946B
Authority
CN
China
Prior art keywords
tower
section
rectifying
rectifying tower
reaction
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.)
Active
Application number
CN2010101459420A
Other languages
English (en)
Other versions
CN101786946A (zh
Inventor
叶子茂
张忠良
张文祥
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.)
Jiangsu Kaimao Chemical Technology Co., Ltd.
Original Assignee
Jiangsu Hengmao Machine Manufacture Co Ltd
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 Jiangsu Hengmao Machine Manufacture Co Ltd filed Critical Jiangsu Hengmao Machine Manufacture Co Ltd
Priority to CN2010101459420A priority Critical patent/CN101786946B/zh
Publication of CN101786946A publication Critical patent/CN101786946A/zh
Application granted granted Critical
Publication of CN101786946B publication Critical patent/CN101786946B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明涉及甲缩醛的生产领域,尤其是一种甲缩醛的制备装置,具有精馏塔,精馏塔自下而上依次包括精馏塔塔底段、精馏塔丝网填料段和精馏塔塔顶段,精馏塔上连接有反应塔,反应塔自下而上依次包括反应塔塔底段、气液分离的反应塔丝网填料段、催化剂填料段和反应塔塔顶段,精馏塔与反应塔是通过精馏塔塔底段与反应塔塔顶段相连进行连接的,反应塔的催化剂填料段上连接有固定床触媒反应器,精馏塔塔顶段连接有冷凝器,精馏塔通过连接在其上的冷凝器连接回流罐。由于本发明的反应塔与精馏塔分开,降低了催化剂填料的高度,使得催化剂再生变得更为方便,有利于提高产品收率,降低了塔的高度,制造和安装容易进行,减小了安全风险。

Description

甲缩醛的制备装置
技术领域
本发明涉及甲缩醛的生产领域,尤其是一种甲缩醛的制备装置。
背景技术
甲缩醛,为微具气味的无色透明液体,能与多种试剂混合,是合成聚甲醛等的重要化工原料,在电子电器、运输、建筑领域、医药、农药和橡胶等行业得到广泛应用。甲缩醛作为一种环保型无苯溶剂,由于其具有的独特理化性能,即良好的溶解性、低沸点、与水相容性好,能广泛用于化妆品、家庭用品、工业汽车用品、杀虫剂、皮革上光剂、橡胶工业、油漆、油墨、鞋用胶粘剂、电子设备清洁剂、彩带配方、空气清新剂配方等产品中,今年来发展很快,尤其是在气雾剂领域展现了很好的应用发展前景。
近年来,在甲缩醛的生产工艺上一直沿用硫酸法,由于硫酸的腐蚀性非常强,导致设备的腐蚀非常严重。为了解决老生产方法的弊病和配合甲缩醛装置,开发了催化精馏法合成甲缩醛,催化剂采用固体树脂代替原来的硫酸,从根本上解决了设备腐蚀的问题。但是一些杂质离子(Fe3+、Mn2+等)易导致树脂催化剂活性降低,影响产品收率。为了保证原料拥有较高的转化率,一般不定期对催化剂进行酸洗再生。即往含有树脂催化剂填料的塔内喷淋盐酸溶液,盐酸溶液润湿催化剂填料,使催化剂填料表面杂质溶解并从塔底排污口排出,从而使催化剂保持较高的活性。同时催化精馏法中的催化剂和丝网填料均填充在一个塔(反应精馏塔)内,致使塔高达约40m。如此高度给催化剂酸洗再生带来不便,对塔的安全也提出了更高的要求,增加了塔的制造成本。
发明内容
本发明要解决的技术问题是:为了解决上述存在的缺点与不足,提供一种甲缩醛的制备装置。
本发明解决其技术问题所采用的技术方案是:甲缩醛的制备装置,具有精馏塔,精馏塔自下而上依次包括精馏塔塔底段、精馏塔丝网填料段和精馏塔塔顶段,精馏塔上连接有反应塔,反应塔自下而上依次包括反应塔塔底段、气液分离的反应塔丝网填料段、催化剂填料段和反应塔塔顶段,精馏塔与反应塔是通过精馏塔塔底段与反应塔塔顶段相连进行连接的,反应塔的催化剂填料段上连接有固定床触媒反应器,精馏塔塔顶段连接有冷凝器,精馏塔通过连接在其上的冷凝器连接回流罐。甲醇和甲醛在固定床触媒反应器内反应,生成含有甲缩醛的混合液,混合液通过反应塔和精馏塔进行气液分离,气体通过冷凝器冷凝后进入回流罐进行甲缩醛成品采出。
精馏塔丝网填料段分为三段,自下而上分别为第一丝网填料段、第二丝网填料段和第三丝网填料段,使得气液分离的更彻底。
本发明的有益效果是,本发明的甲缩醛的制备装置,由于本发明的反应塔与精馏塔分开,降低了催化剂填料的高度,使得催化剂再生变得更为方便,有利于提高产品收率,降低了塔的高度,制造和安装容易进行,减小了安全风险。
附图说明
下面结合附图和实施例对本发明进一步说明。
图1是本发明的结构示意图。
图中1、精馏塔,11、精馏塔塔底段,12、精馏塔丝网填料段,13、精馏塔塔顶段,2、反应塔,21、反应塔塔底段,22、反应塔丝网填料段,23、催化剂填料段,24、反应塔塔顶段,3、固定床触媒反应器,4、冷凝器,5、回流罐。
具体实施方式
现在结合附图对本发明作进一步详细的说明。这些附图均为简化的示意图,仅以示意方式说明本发明的基本结构,因此其仅显示与本发明有关的构成。
如图1所示的甲缩醛的制备装置,具有精馏塔1,精馏塔1自下而上依次包括精馏塔塔底段11、精馏塔丝网填料段12和精馏塔塔顶段13,精馏塔1上连接有反应塔2,反应塔2自下而上依次包括反应塔塔底段21、气液分离的反应塔丝网填料段22、催化剂填料段23和反应塔塔顶段24,精馏塔1与反应塔2是通过精馏塔塔底段11与反应塔塔顶段24相连进行连接的,反应塔2的催化剂填料段23上连接有固定床触媒反应器3,精馏塔塔顶段13连接有冷凝器4,精馏塔1通过连接在其上的冷凝器4连接回流罐5。
将工业品甲醇和甲醛溶液分别用泵打入固定床触媒反应器3中,控制固定床触媒反应器3内的温度在40℃~60℃之间,使得反应器内进行液相反应,生成含有甲缩醛、甲醇及水的混合液。混合液直接送入反应塔2,使得混合液中未反应的甲醇和甲醛进一步反应生成含甲缩醛的混合液,同时混合液在反应塔2底部的再沸器热媒蒸汽加热作用下,形成气液两相,气液两相通过丝网填料时达到平衡并产生初步分离,使得气体部分在塔顶富集,液体部分在塔底的塔釜有较高的浓度。塔底的塔釜废水送至甲醛装置进行回收利用,塔顶的气体送入精馏塔1底部,气体在精馏塔1内有上升的过程,首先气体在精馏塔1的底部,随着上升的过程,经过精馏塔1的丝网填料时与塔顶下来的回流液充分接触达到平衡并产生分离,使得塔顶部产出的为甲缩醛及甲醇共沸物,留在精馏塔1底部的积液用泵打入反应塔2顶部进行循环利用。甲缩醛及甲醇共沸物送入冷凝器4进行冷凝,冷凝后送入回流罐5,回流罐5中的一部分液体通过精馏塔1回流泵打入精馏塔1内进行循环利用,一部分液体形成成品产出,由于部分液体回流至塔顶,使得塔顶余量的重组分被压下,提高甲缩醛的纯度。
由于反应塔2内需要进行进一步的反应,故而反应塔2内的催化剂使用频繁,为了保持催化剂的高活性率,需要不定期对催化剂进行酸洗再生,即向反应塔2喷淋盐酸溶液,使催化剂表面杂质溶解。
由于本发明的反应塔2与精馏塔1分开,降低了催化剂填料的高度,使得催化剂再生变得更为方便,有利于提高产品收率,降低了塔的高度,制造和安装容易进行,减小了安全风险。
以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。

Claims (2)

1.一种甲缩醛的制备装置,具有精馏塔(1),其特征是:精馏塔(1)自下而上依次包括精馏塔塔底段(11)、精馏塔丝网填料段(12)和精馏塔塔顶段(13),精馏塔上连接有反应塔(2),反应塔(2)自下而上依次包括反应塔塔底段(21)、气液分离的反应塔丝网填料段(22)、催化剂填料段(23)和反应塔塔顶段(24),精馏塔(1)与反应塔(2)是通过精馏塔塔底段(11)与反应塔塔顶段(24)相连进行连接的,反应塔(2)的催化剂填料段(23)上连接有固定床触媒反应器(3),精馏塔(1)塔顶段连接有冷凝器(4),精馏塔(1)通过连接在其上的冷凝器(4)连接有回流罐(5)。
2.根据权利要求1所述的甲缩醛的制备装置,其特征是:所述的精馏塔丝网填料段(12)分为三段,自下而上分别为第一丝网填料段、第二丝网填料段和第三丝网填料段。
CN2010101459420A 2010-04-01 2010-04-01 甲缩醛的制备装置 Active CN101786946B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010101459420A CN101786946B (zh) 2010-04-01 2010-04-01 甲缩醛的制备装置

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010101459420A CN101786946B (zh) 2010-04-01 2010-04-01 甲缩醛的制备装置

Publications (2)

Publication Number Publication Date
CN101786946A CN101786946A (zh) 2010-07-28
CN101786946B true CN101786946B (zh) 2012-12-12

Family

ID=42530345

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010101459420A Active CN101786946B (zh) 2010-04-01 2010-04-01 甲缩醛的制备装置

Country Status (1)

Country Link
CN (1) CN101786946B (zh)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068945B (zh) * 2010-12-15 2012-11-21 天津大学 用于甲缩醛分离提纯的反应精馏装置和方法
CN103657129A (zh) * 2013-12-03 2014-03-26 惠州市利而安化工有限公司 带有溶剂加入口的甲缩醛精馏塔
CN103657130B (zh) * 2013-12-03 2015-09-09 惠州市利而安化工有限公司 外置反应器式甲缩醛精馏塔
CN104211586B (zh) * 2014-01-06 2015-10-14 山东辰信新能源有限公司 通过催化剂的在线再生实现连续制备甲缩醛的方法
CN103896747A (zh) * 2014-04-08 2014-07-02 江苏凯茂石化科技有限公司 一种高浓度甲缩醛背包式循环生产工艺装置
CN104193598A (zh) * 2014-08-13 2014-12-10 山东滨州新天阳化工有限责任公司 一种多回流环保型甲缩醛制备工艺
CN104230676A (zh) * 2014-08-13 2014-12-24 山东滨州新天阳化工有限责任公司 一种甲缩醛的制备工艺

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0570719A1 (en) * 1992-04-24 1993-11-24 Showa Denko Kabushiki Kaisha Process for producing acetaldehyde dimethylacetal
CN201660571U (zh) * 2010-04-01 2010-12-01 江苏恒茂机械制造有限公司 一种甲缩醛的制备装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0570719A1 (en) * 1992-04-24 1993-11-24 Showa Denko Kabushiki Kaisha Process for producing acetaldehyde dimethylacetal
CN201660571U (zh) * 2010-04-01 2010-12-01 江苏恒茂机械制造有限公司 一种甲缩醛的制备装置

Also Published As

Publication number Publication date
CN101786946A (zh) 2010-07-28

Similar Documents

Publication Publication Date Title
CN101786946B (zh) 甲缩醛的制备装置
CN102371079B (zh) 高浓度甲缩醛加压精馏工艺及制备装置
US20060178524A1 (en) Method and plant for the manufacture of carboxylic acid ester by means of a reactive distillation
CN101863746A (zh) 甲缩醛的生产工艺及装置
CN110862301B (zh) 一种仲丁醇的精制方法及装置
CN101092337A (zh) 反应精馏和萃取结合制备二甲氧基甲烷的方法
CN102372610B (zh) 高浓度甲缩醛萃取精馏工艺及制备装置
CN101613259A (zh) 电子级丙二醇甲醚的制备方法
CN106699552A (zh) 一种热泵分隔壁反应精馏塔生产乙酸异丙酯的方法
CN101362692A (zh) 一种生产三氟乙酸异丙酯的工艺方法及装置
CN201686631U (zh) 甲缩醛的生产装置
CN101219950B (zh) 一种利用醋酸甲酯和正丁醇的酯交换反应制备醋酸正丁酯的设备和方法
CN110218151A (zh) 一种塔釜闪蒸式热泵反应精馏制备丙酸丙酯的装置和方法
CN110613946B (zh) 一种合成草酸二乙酯的背包反应精馏装备及其工艺
CN102942460B (zh) 一种不饱和缩醛的制备方法
CN101186575B (zh) 一种醋酸甲酯催化精馏水解工艺
CN110423197B (zh) 一种利用低浓度乙二醇生产乙二醇双乙酸酯的装置和方法
CN106883112B (zh) 一种巴豆醛的改进生产工艺
CN201660571U (zh) 一种甲缩醛的制备装置
CN201755420U (zh) 甲缩醛的一塔生产装置
CN102190636B (zh) 氯丙烯环化制环氧氯丙烷的方法
CN101481304B (zh) 一种甲酸甲酯水解制甲酸的工艺
CN107501093B (zh) 一种分隔壁反应精馏塔生产乙二醇二乙酸酯的设备及方法
CN110483282B (zh) 一种生产高浓度乙二醇双乙酸酯的装置和方法
CN201755419U (zh) 高浓度甲缩醛加压精馏制备装置

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: JIANGSU KAIMAO CHEMICAL TECHNOLOGY CO., LTD.

Free format text: FORMER OWNER: JIANGSU HENGMAO MACHINERY MANUFACTURE CO., LTD.

Effective date: 20140430

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 213169 CHANGZHOU, JIANGSU PROVINCE TO: 214000 WUXI, JIANGSU PROVINCE

TR01 Transfer of patent right

Effective date of registration: 20140430

Address after: Xuelang Street Ge Dai Binhu District of Jiangsu Province in 214000 communities in Wuxi City

Patentee after: Jiangsu Kaimao Chemical Technology Co., Ltd.

Address before: 213169, Jiangsu province Changzhou city Wujin District snow town industrial concentration area

Patentee before: Jiangsu Hengmao Machine Manufacture Co., Ltd.

PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Methylal preparation device

Effective date of registration: 20141028

Granted publication date: 20121212

Pledgee: Jiangsu Wujin credit re Company limited by guarantee

Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd.

Registration number: 2014990000897

PLDC Enforcement, change and cancellation of contracts on pledge of patent right or utility model
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20151110

Granted publication date: 20121212

Pledgee: Jiangsu Wujin credit re Company limited by guarantee

Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd.

Registration number: 2014990000897

PLDC Enforcement, change and cancellation of contracts on pledge of patent right or utility model
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Methylal preparation device

Effective date of registration: 20151126

Granted publication date: 20121212

Pledgee: Jiangsu Wujin credit re Company limited by guarantee

Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd.

Registration number: 2015990001050

PLDC Enforcement, change and cancellation of contracts on pledge of patent right or utility model
PC01 Cancellation of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20170608

Granted publication date: 20121212

Pledgee: Jiangsu Wujin credit Company limited by guarantee

Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd.

Registration number: 2015990001050

PM01 Change of the registration of the contract for pledge of patent right

Change date: 20170608

Registration number: 2015990001050

Pledgee after: Jiangsu Wujin credit Company limited by guarantee

Pledgee before: Jiangsu Wujin credit re Company limited by guarantee

PM01 Change of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Methylal preparation device

Effective date of registration: 20170622

Granted publication date: 20121212

Pledgee: Jiangsu Wujin credit Company limited by guarantee

Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd.

Registration number: 2017990000474

PP01 Preservation of patent right
PP01 Preservation of patent right

Effective date of registration: 20180411

Granted publication date: 20121212

PD01 Discharge of preservation of patent
PD01 Discharge of preservation of patent

Date of cancellation: 20181011

Granted publication date: 20121212

PP01 Preservation of patent right
PP01 Preservation of patent right

Effective date of registration: 20181219

Granted publication date: 20121212

PD01 Discharge of preservation of patent

Date of cancellation: 20211219

Granted publication date: 20121212

PD01 Discharge of preservation of patent