CN104341337A - 一种吡啶盐成品的脱色方法 - Google Patents

一种吡啶盐成品的脱色方法 Download PDF

Info

Publication number
CN104341337A
CN104341337A CN201410501498.XA CN201410501498A CN104341337A CN 104341337 A CN104341337 A CN 104341337A CN 201410501498 A CN201410501498 A CN 201410501498A CN 104341337 A CN104341337 A CN 104341337A
Authority
CN
China
Prior art keywords
finished product
pyridinium
methanol
pyridinium salt
hour
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.)
Granted
Application number
CN201410501498.XA
Other languages
English (en)
Other versions
CN104341337B (zh
Inventor
赵金刚
贺玉
杨志健
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.)
Anhui Jinhe Industrial Co Ltd
Original Assignee
Anhui Jinhe Industrial 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 Anhui Jinhe Industrial Co Ltd filed Critical Anhui Jinhe Industrial Co Ltd
Priority to CN201410501498.XA priority Critical patent/CN104341337B/zh
Publication of CN104341337A publication Critical patent/CN104341337A/zh
Application granted granted Critical
Publication of CN104341337B publication Critical patent/CN104341337B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/127—Preparation from compounds containing pyridine rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
    • C07D213/18—Salts thereof

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pyridine Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明涉及一种吡啶盐成品的脱色方法，包括以下步骤：1）将需要脱色的吡啶盐成品与甲醇按照1:1.5的重量比投入反应釜内，升温至50℃搅拌半小时确认物料完结溶解后，再加入重量为吡啶盐成品的1%的活性炭继续搅拌半小时进行脱色；2）脱色过后，用压滤机将活性炭完全压出，将滤液送入蒸馏釜，蒸馏回收甲醇；3）蒸干甲醇后，加入乙醇进行重结晶，离心出成品后，烘干即可得高品质产品。用本发明的方法对吡啶盐进行脱色，生产操作过程相对安全，工作环境明显改善，而且甲醇可以回收利用，相对消耗较少。

Description

一种吡啶盐成品的脱色方法
技术领域
 本发明属于化工脱色技术领域，特别涉及一种吡啶盐成品脱色的方法。
背景技术
现有吡啶盐成品脱色工艺是用氯化亚砜氧化脱色，需要的氯化亚砜用量是吡啶盐成品的2~3倍，因此要消耗大量的氯化亚砜，用过的氯化亚砜不能回收利用，并且要加液碱处理后才能进行排放，氧化脱色过程会产生氯化氢、硫化氢等酸性气体，生产过程操作环境差、危险度高。
发明内容
本发明就是要解决现有技术中操作环境差、危险性高、成品消耗高的问题，提供一种吡啶盐成品的脱色方法。
本发明的技术方案如下 ：
一种吡啶盐成品的脱色方法，其特征在于包括以下步骤：
1）将需要脱色的吡啶盐成品与甲醇按照1:1.5的重量比投入反应釜内，升温至50℃搅拌半小时确认物料完结溶解后，再加入重量为吡啶盐成品的1%的活性炭继续搅拌半小时进行脱色；
2）脱色过后，用压滤机将活性炭完全压出，将滤液送入蒸馏釜，蒸馏回收甲醇；
3）蒸干甲醇后，加入乙醇进行重结晶，离心出成品后，烘干即可得高品质产品。
本发明的优点在于：
用本发明的方法对吡啶盐进行脱色，生产操作过程相对安全，工作环境明显改善，而且甲醇可以回收利用，相对消耗较少。
附图说明
 图1是本发明的工艺流程图。
具体实施方式
向5000L带夹套的搪玻璃反应釜内，投入500kg吡啶盐成品、750kg甲醇，升温至50℃搅拌0.5小时，再加入5kg活性炭，继续搅拌0.5小时后，用压滤机将活性炭压出，将滤液送入蒸馏釜，在0.09MPa、35℃下蒸馏回收甲醇，待甲醇蒸干后，加入600kg无水乙醇，升温至50℃保温2小时后移至结晶釜降温结晶，然后用离心机甩料，得湿品后，烘干可得含量99.5%成品约450kg。

Claims (1)

1.一种吡啶盐成品的脱色方法，其特征在于包括以下步骤：
1）将需要脱色的吡啶盐成品与甲醇按照1:1.5的重量比投入反应釜内，升温至50℃搅拌半小时确认物料完结溶解后，再加入重量为吡啶盐成品的1%的活性炭继续搅拌半小时进行脱色；
2）脱色过后，用压滤机将活性炭完全压出，将滤液送入蒸馏釜，蒸馏回收甲醇；
3）蒸干甲醇后，加入乙醇进行重结晶，离心出成品后，烘干即可得高品质产品。
CN201410501498.XA 2014-09-27 2014-09-27 一种吡啶盐成品的脱色方法 Active CN104341337B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410501498.XA CN104341337B (zh) 2014-09-27 2014-09-27 一种吡啶盐成品的脱色方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410501498.XA CN104341337B (zh) 2014-09-27 2014-09-27 一种吡啶盐成品的脱色方法

Publications (2)

Publication Number Publication Date
CN104341337A true CN104341337A (zh) 2015-02-11
CN104341337B CN104341337B (zh) 2017-03-15

Family

ID=52497869

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410501498.XA Active CN104341337B (zh) 2014-09-27 2014-09-27 一种吡啶盐成品的脱色方法

Country Status (1)

Country Link
CN (1) CN104341337B (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105800828A (zh) * 2016-04-27 2016-07-27 滨海明鸿精细化工有限公司 一种废水中吡啶硫酮钠的回收方法
CN110642780A (zh) * 2019-09-30 2020-01-03 安徽金禾实业股份有限公司 一种提纯黄色吡啶盐酸盐的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102344411A (zh) * 2011-08-01 2012-02-08 宜兴市新宇化工有限公司 一种制备2，6-二甲氧基-3，5-二氨基吡啶盐酸盐的方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102344411A (zh) * 2011-08-01 2012-02-08 宜兴市新宇化工有限公司 一种制备2，6-二甲氧基-3，5-二氨基吡啶盐酸盐的方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105800828A (zh) * 2016-04-27 2016-07-27 滨海明鸿精细化工有限公司 一种废水中吡啶硫酮钠的回收方法
CN105800828B (zh) * 2016-04-27 2019-07-23 滨海明鸿精细化工有限公司 一种废水中吡啶硫酮钠的回收方法
CN110642780A (zh) * 2019-09-30 2020-01-03 安徽金禾实业股份有限公司 一种提纯黄色吡啶盐酸盐的方法
CN110642780B (zh) * 2019-09-30 2022-10-18 安徽金禾实业股份有限公司 一种提纯黄色吡啶盐酸盐的方法

Also Published As

Publication number Publication date
CN104341337B (zh) 2017-03-15

Similar Documents

Publication Publication Date Title
Wu et al. Effect of dimethyl sulfoxide on ionic liquid 1-ethyl-3-methylimidazolium acetate pretreatment of eucalyptus wood for enzymatic hydrolysis
CN103787874A (zh) 一种苯甲酰氯的制备工艺
CN109721471B (zh) 一种从生产生物柴油的副产物中提纯甘油的方法
CN102875587B (zh) 一种利用多硫化钠合成含硫硅烷偶联剂的方法
Li et al. Simultaneous isomerization and reactive extraction of biomass sugars for high yield production of ketose sugars
CN103314013A (zh) 同时水解和氢化纤维素
CN103319324B (zh) 一种碱-氧氧化褐煤制备苯羧酸的方法
CN104341337A (zh) 一种吡啶盐成品的脱色方法
JP6587640B2 (ja) カルボン酸のα−オレフィンへの変換
RU2016128516A (ru) Находящиеся под давлением сырьевые смеси, содержащие неочищенные ароматические карбоновые кислоты
CA2763332A1 (en) Levulinic acid from fungal biomass
CN102795989B (zh) 十二烷二酸精制方法
Karnjanakom et al. A facile way for sugar transformation catalyzed by carbon-based Lewis-Brønsted solid acid
CN107032308A (zh) 一种烷基化废硫酸资源化回收方法
CN102827041B (zh) 一种对甲砜基苯甲醛的制备方法
CN104529766A (zh) 一种季戊四醇三硬脂酸酯的制备方法
CN108084008B (zh) 一种丙酮一步法合成甲基异丁基酮工艺的开工方法
CN109721566B (zh) 一种1-（4-吗啉苯基）-1-丁酮的制备方法
CN103880603A (zh) 一种催化制备苯乙烯化苯酚的方法
CN103951557A (zh) 一种以无机碱为催化剂制备非诺贝特酸的方法
CN112313365A (zh) 阳极电解液部分催化的hmf生产
CN103804174A (zh) 一种有机酸的精制方法
CN102994223A (zh) 用磷酸对小机榨菜籽饼浸出油进行脱色的方法
CN102249957B (zh) 用2b油磺化生产2b酸的方法
CN101643246A (zh) 一种铼酸铵除杂提纯法

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