CN108727228A - A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes - Google Patents
A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes Download PDFInfo
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- CN108727228A CN108727228A CN201710990581.1A CN201710990581A CN108727228A CN 108727228 A CN108727228 A CN 108727228A CN 201710990581 A CN201710990581 A CN 201710990581A CN 108727228 A CN108727228 A CN 108727228A
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- air blowing
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- oxygen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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Abstract
The present invention is a kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), is comprised the step of：(1) preparation of production system：Prepare eight 5m3Feed inlet is arranged in stills for air blowing, all stills for air blowing bottoms, and discharge port is arranged in top；Seven are connected, one spare, and spare stills for air blowing come into operation when carrying production or other oxidation furnaces checking maintenances, concatenated seven stills for air blowing label 1#-7# successively, oxygen pipeline is arranged in 1#-7# stills for air blowing bottom, and 3# stills for air blowing bottom, which increases, mends ammonia pipeline, and 7# stills for air blowing connect transfer tank；(2) continuous production.The present invention, raw material pass through concatenated stills for air blowing gradual reaction, continue to provide kinetic energy for reaction wherein increasing and mending ammonia pipeline, multiple spot is added oxygen, keeps reaction more abundant, improve production efficiency；This technique reduces frequent driving and parking, without frequent heating, cooling process, substantially saves energy consumption (steam consumption), improves product yield, reduce human cost.
Description
Technical field
The present invention relates to vulcanization accelerator diphenylguanidine (DPG) synthesis field more particularly to a kind of vulcanization accelerator diphenylguanidine
(DPG) continuous production processes.
Background technology
Vulcanization accelerator can improve curingprocess rate, control the temperature in sulfidation, shorten vulcanization time, play simultaneously
The effect for reducing sulphur cost, has obtained very extensive application in rubber production of today.Diphenylguanidine (DPG) is a kind of sulphur
Change accelerating agent, belongs to medium accelerator, can be used as the activator of thiazoles thiuram and sulfenamide type accelerators.With accelerating agent
Simultaneously the used time is used for continuous vulcanization by DM, TMTD.There is anti-aging property.It is common to natural gum and rubber polymer, is not suitable for latex.Mainly
For manufacturing the mechanical rubber goods such as tire, offset plate, rubber overshoes.
Currently, Workshop Production DPG products use one-pot reaction, is put into and beaten using quantitative CA, ammonium hydroxide and catalyst
Tank is starched, then enters stills for air blowing after being sufficiently mixed, is heated up, into oxygen oxidation process, reaction total duration 4-6 hours, reaction is qualified
Carry out the blowing water-washing process of next step again afterwards.
Existing production technology has the drawback that：React insufficient, production efficiency is low；It needs frequently to open work(closing oxygen
Change kettle, frequently carries out heating, cooling, large steam consumption, energy consumption is very big, and product yield is low, and human cost is very high.
For this purpose, designing a kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), problem above is solved.
Invention content
The present invention is to overcome the above deficiency, provides a kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), including
The step of have：
(1) preparation of production system：
Prepare eight 5m3Feed inlet is arranged in stills for air blowing, all stills for air blowing bottoms, and discharge port is arranged in top；Seven are connected,
One spare, and spare stills for air blowing come into operation when carrying production or other oxidation furnaces checking maintenances, and concatenated seven stills for air blowing are marked successively
Oxygen pipeline is arranged in number 1#-7#, 1#-7# stills for air blowing bottom, and 3# stills for air blowing bottom, which increases, mends ammonia pipeline, and 7# stills for air blowing connect transfer
Tank；
(2) continuous production：
By N, N`- rhenocure CAs (CA), catalyst, 25% concentration ammonium hydroxide composition mixture with 0.33MPa pressure
And 5.17m3The charging rate of/h enters 1# stills for air blowing from 1# stills for air blowing bottom feed inlet, goes out from 1# stills for air blowing top discharge mouths
Come after from the bottom feed inlet of next stills for air blowing enter next stills for air blowing, until 7# stills for air blowing discharging finish, output DPG and
Into transfer tank；
Ammonia is mended with the speed of 300L/h from the ammonia pipeline of mending of 3# stills for air blowing bottom；
It is that all stills for air blowing bottoms convey oxygen from oxygen pipeline, from 1# stills for air blowing to 7# stills for air blowing, successively decrease oxygen successively
Inlet amount；Per hour by analyzing personnel from 3# stills for air blowing and 7# stills for air blowing discharging pipeline sample detection purity.
The beneficial effects of the invention are as follows：
A kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG) of the present invention, raw material pass through concatenated oxygen
Change kettle gradual reaction, continues to provide kinetic energy for reaction wherein increasing and mending ammonia pipeline, multiple spot is added oxygen, keeps reaction more abundant, carry
High production efficiency；This technique reduces frequent driving and parking, without frequent heating, cooling process, substantially saves energy consumption (steam
Consumption), product yield is improved, human cost is reduced.
Specific implementation mode
It is described in detail below with reference to the embodiment of the present invention.
A kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), comprise the step of：
(1) preparation of production system：
Prepare eight 5m3Feed inlet is arranged in stills for air blowing, all stills for air blowing bottoms, and discharge port is arranged in top；Seven are connected,
One spare, and spare stills for air blowing come into operation when carrying production or other oxidation furnaces checking maintenances, and concatenated seven stills for air blowing are marked successively
Oxygen pipeline is arranged in number 1#-7#, 1#-7# stills for air blowing bottom, and 3# stills for air blowing bottom, which increases, mends ammonia pipeline, and 7# stills for air blowing connect transfer
Tank；
(2) continuous production：
By N, N`- rhenocure CAs (CA), catalyst, 25% concentration ammonium hydroxide composition mixture with 0.33MPa pressure
And 5.17m3The charging rate of/h enters 1# stills for air blowing from 1# stills for air blowing bottom feed inlet, goes out from 1# stills for air blowing top discharge mouths
Come after from the bottom feed inlet of next stills for air blowing enter next stills for air blowing, until 7# stills for air blowing discharging finish, output DPG and
Into transfer tank；
Ammonia is mended with the speed of 300L/h from the ammonia pipeline of mending of 3# stills for air blowing bottom；
It is that all stills for air blowing bottoms convey oxygen from oxygen pipeline, from 1# stills for air blowing to 7# stills for air blowing, successively decrease oxygen successively
Inlet amount；Per hour by analyzing personnel from 3# stills for air blowing and 7# stills for air blowing discharging pipeline sample detection purity.
Embodiment：
A kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), comprise the step of：
(1) preparation of production system：
Prepare eight 5m3Feed inlet is arranged in stills for air blowing, all stills for air blowing bottoms, and discharge port is arranged in top；Seven are connected,
One spare, and spare stills for air blowing come into operation when carrying production or other oxidation furnaces checking maintenances, and concatenated seven stills for air blowing are marked successively
Oxygen pipeline is arranged in number 1#-7#, 1#-7# stills for air blowing bottom, and 3# stills for air blowing bottom, which increases, mends ammonia pipeline, and 7# stills for air blowing connect transfer
Tank；
(2) continuous production：
The N of 700kg, N`- rhenocure CA (CA), 800g catalyst, 4640L 25% concentration ammonium hydroxide mixture with
0.33MPa pressure and 5.17m3The charging rate of/h enters 1# stills for air blowing from bottom feed inlet, after top discharge mouth comes out
Enter next stills for air blowing from the bottom feed inlet of next stills for air blowing, until the discharging of 7# stills for air blowing finishes, into transfer tank；
Ammonia is mended with the speed of 300L/h from the ammonia pipeline of mending of 3# stills for air blowing bottom, increases reaction kinetic energy；
It is that all stills for air blowing bottoms convey oxygen from oxygen pipeline, balancing oxygen total feed according to actual production exists
137kg/h, due to reacting early period, reaction is violent, and when bottom leads to oxygen, each kettle successively decreases oxygen feeding amount 1# stills for air blowing into oxygen successively
32kg/h, 2# stills for air blowing are 28kg/h, and 3# stills for air blowing are 24kg/h, and 4# stills for air blowing are 20kg/h, and 5# stills for air blowing are 16kg/h, 6#
Stills for air blowing are 12kg/h, and 7# stills for air blowing are 5kg/h；Reaction mass is about 6.4 hours by the stills for air blowing residence time；Per hour by
Analysis personnel discharge pipeline sample detection purity from 3# stills for air blowing and 7# stills for air blowing.
Reaction pattern originally puts into stills for air blowing 8, and every batch of puts into 425kgCA, and production 32 batches, the total input amounts of CA are daily
13.6 tons, Gross Output DPG is 12.16 tons, after being changed to continuous production, can greatly improve production efficiency, the daily total input amounts of CA
It it is 16.8 tons, Gross Output product is 15.02 tons, can improve 24% production efficiency.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of continuous production processes of vulcanization accelerator diphenylguanidine (DPG), which is characterized in that comprise the step of：
(1) preparation of production system：
Prepare eight 5m3Feed inlet is arranged in stills for air blowing, all stills for air blowing bottoms, and discharge port is arranged in top；Seven are connected, one
Spare, spare stills for air blowing are proposing production or whens other oxidation furnaces checking maintenances comes into operation, concatenated seven stills for air blowing label 1#- successively
Oxygen pipeline is arranged in 7#, 1#-7# stills for air blowing bottom, and 3# stills for air blowing bottom, which increases, mends ammonia pipeline, and 7# stills for air blowing connect transfer tank；
(2) continuous production：
By N, N`- rhenocure CAs, catalyst, 25% concentration ammonium hydroxide composition mixture with 0.33MPa pressure and
5.17m3The charging rate of/h enters 1# stills for air blowing from 1# stills for air blowing bottom feed inlet, after 1# stills for air blowing top discharge mouths come out
Enter next stills for air blowing from the bottom feed inlet of next stills for air blowing, until the discharging of 7# stills for air blowing finishes, output DPG and entrance
Transfer tank；
Ammonia is mended with the speed of 300L/h from the ammonia pipeline of mending of 3# stills for air blowing bottom；
From oxygen pipeline be all stills for air blowing bottoms convey oxygen, from 1# stills for air blowing to 7# stills for air blowing, the oxygen that successively decreases successively into
Doses；Per hour by analyzing personnel from 3# stills for air blowing and 7# stills for air blowing discharging pipeline sample detection purity.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990581.1A CN108727228A (en) | 2017-10-23 | 2017-10-23 | A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990581.1A CN108727228A (en) | 2017-10-23 | 2017-10-23 | A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes |
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| CN108727228A true CN108727228A (en) | 2018-11-02 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB199354A (en) * | 1922-06-19 | 1924-07-07 | Naugatuck Chem Co | Improvements in or relating to processes for the manufacture of diphenyl guanidine |
| US4898978A (en) * | 1985-01-17 | 1990-02-06 | Akzo N.V. | Process for the preparation of N,N'-disubstituted guanidines |
| CN102363601A (en) * | 2011-09-20 | 2012-02-29 | 科迈化工股份有限公司 | Method for producing rubber accelerator DGP by using hydrogen peroxide as oxidant |
| CN103804161A (en) * | 2012-11-06 | 2014-05-21 | 中国石油化工股份有限公司 | Air distribution method in cyclohexane oxidation reaction for cyclohexanone production |
| CN104672109A (en) * | 2013-12-03 | 2015-06-03 | 天津一化化工有限公司 | Production process of rubber accelerator DPG |
| CN105037215A (en) * | 2015-07-16 | 2015-11-11 | 山东阳谷华泰化工股份有限公司 | High-yield environment-friendly oxygen oxidation method for synthesis of accelerator DPG |
| CN105348149A (en) * | 2015-12-15 | 2016-02-24 | 山东尚舜化工有限公司 | Method for improving quality of diphenylguanidine product |
| CN106995390A (en) * | 2017-03-06 | 2017-08-01 | 山东尚舜化工有限公司 | It is a kind of to reduce the method that waste water is produced in accelerator diphenylguanidine production process |
| CN107540577A (en) * | 2016-06-29 | 2018-01-05 | 宁夏海诚电化信息科技有限公司 | A kind of diphenylguanidine PG production technologies |
-
2017
- 2017-10-23 CN CN201710990581.1A patent/CN108727228A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB199354A (en) * | 1922-06-19 | 1924-07-07 | Naugatuck Chem Co | Improvements in or relating to processes for the manufacture of diphenyl guanidine |
| US4898978A (en) * | 1985-01-17 | 1990-02-06 | Akzo N.V. | Process for the preparation of N,N'-disubstituted guanidines |
| CN102363601A (en) * | 2011-09-20 | 2012-02-29 | 科迈化工股份有限公司 | Method for producing rubber accelerator DGP by using hydrogen peroxide as oxidant |
| CN103804161A (en) * | 2012-11-06 | 2014-05-21 | 中国石油化工股份有限公司 | Air distribution method in cyclohexane oxidation reaction for cyclohexanone production |
| CN104672109A (en) * | 2013-12-03 | 2015-06-03 | 天津一化化工有限公司 | Production process of rubber accelerator DPG |
| CN105037215A (en) * | 2015-07-16 | 2015-11-11 | 山东阳谷华泰化工股份有限公司 | High-yield environment-friendly oxygen oxidation method for synthesis of accelerator DPG |
| CN105348149A (en) * | 2015-12-15 | 2016-02-24 | 山东尚舜化工有限公司 | Method for improving quality of diphenylguanidine product |
| CN107540577A (en) * | 2016-06-29 | 2018-01-05 | 宁夏海诚电化信息科技有限公司 | A kind of diphenylguanidine PG production technologies |
| CN106995390A (en) * | 2017-03-06 | 2017-08-01 | 山东尚舜化工有限公司 | It is a kind of to reduce the method that waste water is produced in accelerator diphenylguanidine production process |
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Application publication date: 20181102 |