CN106995390B - A method of it reducing waste water in promotor diphenylguanidine production process and generates - Google Patents
A method of it reducing waste water in promotor diphenylguanidine production process and generates Download PDFInfo
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- CN106995390B CN106995390B CN201710127450.0A CN201710127450A CN106995390B CN 106995390 B CN106995390 B CN 106995390B CN 201710127450 A CN201710127450 A CN 201710127450A CN 106995390 B CN106995390 B CN 106995390B
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- diphenylguanidine
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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 relates to diphenylguanidine production technical fields, particularly disclose a kind of method for reducing waste water generation in promotor diphenylguanidine production process.The method that waste water generates in the reduction promotor diphenylguanidine production process, it is characterised in that: absorb water using the washing water of diphenylguanidine product as with ammonia, be configured to ammonium hydroxide；Ammonium hydroxide, CA and catalyst are put into stills for air blowing, agitating and heating, until oxidation temperature in the kettle starts logical oxygen when being 64 ± 2 DEG C, stops logical oxygen when reacting to terminal.Operation of the present invention is simple, is easy to industrialize, and does not influence on product quality, reduces 60% or more DPG wastewater discharge, greatly reduces waste water yield, alleviate water process pressure, is conducive to environmental protection.
Description
(1) technical field
The present invention relates to diphenylguanidine production technical field, in particular to give up in a kind of reduction promotor diphenylguanidine production process
The method that water generates.
(2) background technique
Promotor diphenylguanidine also known as diphenylguanidine PG, are one of important specieses of thiofide, in natural rubber
Be used as medium accelerator in synthetic rubber, had a good application prospect in traditional rubber products and tire.Production at present
The process of diphenylguanidine PG has the method for lead oxide, sodium cyanide method, Oxygen Catalytic Oxidation method etc., and wherein industrial applications are the widest
General is oxygen catalytic method, but this method generation wastewater flow rate is big, and ammonia-nitrogen content is high, and Water purification brings very big pressure.With
Society development and technology continuous propulsion, to technique, more stringent requirements are proposed, reduce discharge of wastewater, by all round process
Greenization is as strategic objective.
(3) summary of the invention
A kind of in order to compensate for the shortcomings of the prior art, the present invention provides steps simple, energy-saving and environment-friendly reduction promotor
The method that waste water generates in diphenylguanidine production process.
The present invention is achieved through the following technical solutions:
A method of it reducing waste water in promotor diphenylguanidine production process and generates, it is characterised in that: with diphenylguanidine product
Washing water be used as with ammonia absorb water, be configured to ammonium hydroxide；Ammonium hydroxide, CA and catalyst are put into stills for air blowing, agitating and heating, until
Oxidation temperature in the kettle starts logical oxygen when being 64 ± 2 DEG C, stop logical oxygen when reacting to terminal.
The present invention absorbs water using diphenylguanidine washing water as with ammonia, and the ammonia steamed to absorb continuous still prepares one
The ammonium hydroxide for determining concentration heats logical oxygen in stills for air blowing with CA, catalyst and reacts, the useless of diphenylguanidine is effectively reduced as raw material
Water discharge amount.
Diphenylguanidine product washing water absorbs water with ammonia as next batch materials and uses, and does not enter back into mother liquor and is distilled, is dropped
Low wastewater treatment capacity.
More excellent technical solution of the invention are as follows:
The washing water of the diphenylguanidine product is preceding wash water twice, and weight ratio containing ammonia is 5-7%, after twice wash water it is direct
For wash water twice before next batch, it is recycled with this.
The mass concentration of the ammonium hydroxide is 20-24%.
The mol ratio of the ammonium hydroxide and CA are 20-24:1.
The water of the diphenylguanidine oxidation mother liquor is 340-360ml, the total 600ml of washing water twice before diphenylguanidine product, after
The total 400ml of washing water twice.
Operation of the present invention is simple, is easy to industrialize, and does not influence on product quality, reduce DPG wastewater discharge 60% with
On, waste water yield is greatly reduced, water process pressure is alleviated, is conducive to environmental protection.
(4) specific embodiment
Embodiment 1:
CA 60g dry product is added in stills for air blowing, prepares ammonia spirit (ammonia density 23.5%) 500ml, catalysis using clear water
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, clean filter cake with clear water in four times, washing water 600ml washing water 400ml twice with after twice before collecting respectively.
It is dried to obtain diphenylguanidine PG finished product.
Evaporated mother liquor goes out ammonia, and with the preceding 600ml absorbing ammonia of washing water twice, it is real for next group to prepare ammonia mass concentration 20%
It tests.Washing water 400ml is used for before next group experiment wash water twice twice afterwards.
It takes in above-mentioned 20% ammonia solution 510ml of preparation mass concentration investment stills for air blowing, while dry product CA 60g, catalysis is added
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, and washing water 400ml and 200ml clear water are received as washing water twice before this batch twice after taking last consignment of to test
Collection is for matching ammonia.Circuit sequentially use.
Embodiment 2:
CA 60g dry product is added in stills for air blowing, prepares ammonia spirit (ammonia density 23.5%) 500ml, catalysis using clear water
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, clean filter cake with clear water in four times, washing water 600ml washing water 400ml twice with after twice before collecting respectively.
It is dried to obtain diphenylguanidine PG finished product.
Evaporated mother liquor goes out ammonia, and with the preceding 600ml absorbing ammonia of washing water twice, it is real for next group to prepare ammonia mass concentration 22%
It tests.Washing water 400ml is used for before next group experiment wash water twice twice afterwards.
It takes in above-mentioned 22% ammonia solution 490ml of preparation mass concentration investment stills for air blowing, while dry product CA 60g, catalysis is added
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, and washing water 400ml and 200ml clear water are received as washing water twice before this batch twice after taking last consignment of to test
Collection is for matching ammonia.Circuit sequentially use.
Embodiment 3:
CA 60g dry product is added in stills for air blowing, prepares ammonia spirit (ammonia density 23.5%) 500ml, catalysis using clear water
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, clean filter cake with clear water in four times, washing water 600ml washing water 400ml twice with after twice before collecting respectively.
It is dried to obtain diphenylguanidine PG finished product.
Evaporated mother liquor goes out ammonia, and with the preceding 600ml absorbing ammonia of washing water twice, it is real for next group to prepare ammonia mass concentration 24%
It tests.Washing water 400ml is used for before next group experiment wash water twice twice afterwards.
It takes in above-mentioned 24% ammonia solution 485ml of preparation mass concentration investment stills for air blowing, while dry product CA 60g, catalysis is added
Agent 0.1500g is quickly stirred, and is heated to 64 ± 2 DEG C of temperature in the kettle and is started logical oxygen, stops logical oxygen when being reacted to terminal.It filtered
Mother liquor is collected in filter, and washing water 400ml and 200ml clear water are received as washing water twice before this batch twice after taking last consignment of to test
Collection is for matching ammonia.Circuit sequentially use.
Claims (3)
1. a kind of reduce the method that waste water generates in promotor diphenylguanidine production process, it is characterised in that: with diphenylguanidine product
Washing water, which is used as, absorbs water with ammonia, is configured to ammonium hydroxide；Ammonium hydroxide, CA and catalyst are put into stills for air blowing, agitating and heating, until oxygen
Change and start logical oxygen when temperature in the kettle is 64 ± 2 DEG C, stops logical oxygen when reacting to terminal；Before the washing water of the diphenylguanidine product is
Wash water twice, weight ratio containing ammonia be 5-7%, after twice wash water be directly used in front of next batch wash water twice, being recycled with this makes
With；The water of the diphenylguanidine oxidation mother liquor is 340-360ml, the total 600ml of washing water twice before diphenylguanidine product, after water twice
The total 400ml of wash water.
2. according to claim 1 reduce the method that waste water generates in promotor diphenylguanidine production process, it is characterised in that:
The mass concentration of the ammonium hydroxide is 20-24%.
3. according to claim 1 reduce the method that waste water generates in promotor diphenylguanidine production process, it is characterised in that:
The mol ratio of the ammonium hydroxide and CA are 20-24:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127450.0A CN106995390B (en) | 2017-03-06 | 2017-03-06 | A method of it reducing waste water in promotor diphenylguanidine production process and generates |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127450.0A CN106995390B (en) | 2017-03-06 | 2017-03-06 | A method of it reducing waste water in promotor diphenylguanidine production process and generates |
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| Publication Number | Publication Date |
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| CN106995390A CN106995390A (en) | 2017-08-01 |
| CN106995390B true CN106995390B (en) | 2019-03-19 |
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| CN201710127450.0A Active CN106995390B (en) | 2017-03-06 | 2017-03-06 | A method of it reducing waste water in promotor diphenylguanidine production process and generates |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108727228A (en) * | 2017-10-23 | 2018-11-02 | 科迈化工股份有限公司 | A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215272A (en) * | 2008-01-16 | 2008-07-09 | 天津市科迈化工有限公司 | Method of producing rubber vulcanization accelerator DM |
| CN101735171A (en) * | 2009-11-16 | 2010-06-16 | 天津市科迈化工有限公司 | Method for synthesizing thiofide NS by oxygen oxidation method |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205035304U (en) * | 2015-09-25 | 2016-02-17 | 鹤壁市恒力橡塑股份有限公司 | Reduce production system that rubber vulcanization accelerator DPG liquid ammonia consumed |
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- 2017-03-06 CN CN201710127450.0A patent/CN106995390B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215272A (en) * | 2008-01-16 | 2008-07-09 | 天津市科迈化工有限公司 | Method of producing rubber vulcanization accelerator DM |
| CN101735171A (en) * | 2009-11-16 | 2010-06-16 | 天津市科迈化工有限公司 | Method for synthesizing thiofide NS by oxygen oxidation method |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
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