CN104592108A - One-step synthetic process of rubber antioxidant RD - Google Patents
One-step synthetic process of rubber antioxidant RD Download PDFInfo
- Publication number
- CN104592108A CN104592108A CN201310525433.4A CN201310525433A CN104592108A CN 104592108 A CN104592108 A CN 104592108A CN 201310525433 A CN201310525433 A CN 201310525433A CN 104592108 A CN104592108 A CN 104592108A
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- CN
- China
- Prior art keywords
- aniline
- hydrochloric acid
- reaction
- acetone
- raw materials
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- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/04—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to the ring carbon atoms
- C07D215/06—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to the ring carbon atoms having only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, attached to the ring nitrogen atom
Abstract
The invention discloses a one-step synthetic process of a rubber antioxidant RD. The process is as below: using aniline and acetone as raw materials for reaction and hydrochloric acid as a catalyst; reacting aniline with hydrochloric acid in a reaction kettle with a stirrer for synthesis of aniline hydrochloride; conducting condensation reaction on the aniline hydrochloride with an excessive amount of acetone in the reaction kettle with stirrer to generate a polymer; neutralizing hydrochloric acid in the reaction process with sodium hydroxide; recovering acetone and aniline from the water phase in a waste water tower; clarifying the oil phase, conducting continuous dehydration in a flash tank, and steaming to remove aniline; and sending the condensation polymer with aniline removed into a finished product distillation tower for removing a front cut fraction, so as to finally obtain the product of antioxidant RD. Compared with a traditional one-step method, the improved one-step method can timely deprive unreacted raw materials, so that the content of active ingredients (dimer, trimer and tetramer) substantially increases.
Description
Technical field
The invention belongs to anti-aging agent production technical field, be specifically related to a kind of one-step synthesis process of rubber antiager RD.
Background technology
The one-step synthesis process of rubber antiager RD refers to the condensation of raw material, polyreaction is carried out in same reactor, and namely a step obtains product.This technical process is short, equipment is few, cost is low, but in reaction process, can not remove unreacted raw material in time, and cause active constituent content in product lower, foreign matter content is high.
Summary of the invention
The object of the invention is to, provide a kind of one-step synthesis process of rubber antiager RD, the more traditional single stage method of improved single stage method can remove unreacted raw material in time, and effective constituent in product (two, three, the tetramer) content improves greatly.
The one-step synthesis process of rubber antiager RD provided by the invention, with aniline and acetone for reaction raw materials, it is characterized in that, take hydrochloric acid as catalyzer, in with the reactor of agitator, aniline and hydrochloric acid reaction are synthesized aniline salt hydrochloric acid, the aniline salt hydrochloric acid generated carries out polycondensation with excessive acetone again in the reactor of agitator, generate polymkeric substance, hydrochloric acid sodium hydroxide in reaction process neutralizes, aqueous phase and waste water tower reclaim acetone, aniline, after oil phase clarification after flash tank continuously dehydrating, enter steaming aniline and take off aniline, the polycondensate taking off aniline enters into finished product distillation tower again and sloughs front-end volatiles, finally obtain anti-aging agent RD product.
The one-step synthesis process of rubber antiager RD provided by the invention, its beneficial effect is: the more traditional single stage method of improved single stage method can remove unreacted raw material in time, and effective constituent in product (two, three, the tetramer) content improves greatly.
Embodiment
Below in conjunction with an embodiment, the one-step synthesis process of rubber antiager RD provided by the invention is described in detail.
Embodiment
The one-step synthesis process of the rubber antiager RD of the present embodiment, with aniline and acetone for reaction raw materials, it is characterized in that, take hydrochloric acid as catalyzer, in with the reactor of agitator, aniline and hydrochloric acid reaction are synthesized aniline salt hydrochloric acid, the aniline salt hydrochloric acid generated carries out polycondensation with excessive acetone again in the reactor of agitator, generate polymkeric substance, hydrochloric acid sodium hydroxide in reaction process neutralizes, aqueous phase and waste water tower reclaim acetone, aniline, after oil phase clarification after flash tank continuously dehydrating, enter steaming aniline and take off aniline, the polycondensate taking off aniline enters into finished product distillation tower again and sloughs front-end volatiles, finally obtain anti-aging agent RD product.
Claims (1)
1. the one-step synthesis process of a rubber antiager RD, with aniline and acetone for reaction raw materials, it is characterized in that, take hydrochloric acid as catalyzer, in with the reactor of agitator, aniline and hydrochloric acid reaction are synthesized aniline salt hydrochloric acid, the aniline salt hydrochloric acid generated carries out polycondensation with excessive acetone again in the reactor of agitator, generate polymkeric substance, hydrochloric acid sodium hydroxide in reaction process neutralizes, aqueous phase and waste water tower reclaim acetone, aniline, after oil phase clarification after flash tank continuously dehydrating, enter steaming aniline and take off aniline, the polycondensate taking off aniline enters into finished product distillation tower again and sloughs front-end volatiles, finally obtain anti-aging agent RD product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525433.4A CN104592108A (en) | 2013-10-31 | 2013-10-31 | One-step synthetic process of rubber antioxidant RD |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525433.4A CN104592108A (en) | 2013-10-31 | 2013-10-31 | One-step synthetic process of rubber antioxidant RD |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104592108A true CN104592108A (en) | 2015-05-06 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310525433.4A Pending CN104592108A (en) | 2013-10-31 | 2013-10-31 | One-step synthetic process of rubber antioxidant RD |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104592108A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316941A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Method for continuous neutralization and water separation of polycondensation liquid in production process of antioxidant TMQ |
| CN107868042A (en) * | 2016-09-28 | 2018-04-03 | 中国石油化工股份有限公司 | Polycondensation reaction liquid continuously neutralizes, continuously divides the method for water in age resistor TMQ production processes |
| CN109665991A (en) * | 2017-10-16 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of preparation method of anti-aging agent TMQ |
-
2013
- 2013-10-31 CN CN201310525433.4A patent/CN104592108A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316941A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Method for continuous neutralization and water separation of polycondensation liquid in production process of antioxidant TMQ |
| CN107868042A (en) * | 2016-09-28 | 2018-04-03 | 中国石油化工股份有限公司 | Polycondensation reaction liquid continuously neutralizes, continuously divides the method for water in age resistor TMQ production processes |
| CN109665991A (en) * | 2017-10-16 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of preparation method of anti-aging agent TMQ |
| CN109665991B (en) * | 2017-10-16 | 2022-08-23 | 中国石油化工股份有限公司 | Preparation method of anti-aging agent TMQ |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150506 |