CN104672109A - Production process of rubber accelerator DPG - Google Patents

Production process of rubber accelerator DPG Download PDF

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Publication number
CN104672109A
CN104672109A CN201310643889.0A CN201310643889A CN104672109A CN 104672109 A CN104672109 A CN 104672109A CN 201310643889 A CN201310643889 A CN 201310643889A CN 104672109 A CN104672109 A CN 104672109A
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China
Prior art keywords
dpg
tank
section door
open
mother liquor
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Pending
Application number
CN201310643889.0A
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Chinese (zh)
Inventor
张维仁
任树清
岳姝雅
邹燕燕
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TIANJIN YIHUA CHEMICAL CO Ltd
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TIANJIN YIHUA CHEMICAL CO Ltd
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Priority to CN201310643889.0A priority Critical patent/CN104672109A/en
Publication of CN104672109A publication Critical patent/CN104672109A/en
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Abstract

The invention discloses a production process of a rubber accelerator DPG, which comprises the following steps: sequentially putting certain amounts of an accelerator DPTU, a catalyst and prepared qualified ammonium hydroxide into a DPG preparation tank, stirring the obtained mixture, and putting the obtained mixture into a DPG oxidation tank; at certain temperature and pressure, feeding O2 for oxidation; carrying out water washing on the DPG obtained by oxidation, and spin-drying the DPG; and pneumatic drying, and sieving the obtained product, so that a product is obtained. The production process disclosed by the invention has the beneficial effects that the method can improve the yield and purity of the accelerator DPG, improve the yield and the product quality, and reduce the production cost; and rubber products prepared by using the accelerator prepared by using the method are low in impurity content, and the service lives of the rubber products are prolonged.

Description

The production technique of a kind of rubber accelerator DPG
(1) technical field
The present invention relates to a kind of rubber accelerator production technique, particularly relate to the production technique of a kind of rubber accelerator DPG.
(2) background technology
At present, rubber accelerator DPG is one of conventional delayed action accelerator, for natural rubber and synthetical glue, be commonly used for the promoting agent of thiazoles, thiuram and sulfenamide type accelerators, endless vulcanization is can be used for altax, TMTD used time, in chloroprene rubber, this product has the effect of softening agent, peptizer.Mainly for the manufacture of tire, offset plate, sole, mechanicals, hard rubber and thick article.But present rubber accelerator DPG is due to the impact of production technique, productive rate generally maintains about 94%, and purity is about 96%, causes the rubber product foreign matter content produced with this promotor more, and impact uses.Productive rate and purity can be improved on the market, improve output and quality product, reduce production cost, and the production technique of rubber accelerator DPG that the rubber product foreign matter content that the promotor that this method of use is made is produced is low, work-ing life extends is not also found, and awaits exploitation.
(3) summary of the invention
In order to overcome the weak point of existing rubber accelerator production technique, the invention provides the production technique of a kind of rubber accelerator DPG.
Technical scheme of the present invention realizes like this.
The production technique of a kind of rubber accelerator DPG of this programme, concrete steps are as follows:
(1) DPG synthesis:
1. prepare burden
Check whether DPG reactor possesses formal driving condition, and perform the button-up operations fed intake;
Close material-compound tank discharging section door, open the emptying section door of material-compound tank, open vulkacit D PTU feeding cover, drop into 450kg vulkacit D PTU and 500g catalyzer to material-compound tank, finish and namely cover tightly charging opening;
Unlatching joins ammonia pump to the corresponding section door of DPG material-compound tank, starts to squeeze into into aqua ammonia pump to DPG material-compound tank surely to throw ammonia vol 1650L by middle detection;
Start material-compound tank to stir, after evenly. open emptying section door on material-compound tank bottom discharge section door and corresponding DPG reactor, open corresponding section door and corresponding DPG oxidation tank upper feeding section door on material-compound tank dnockout pipeline, start dnockout pump to DPG reactor feed;
Treat that in material-compound tank, material is beaten to the greatest extent, then open into aqua ammonia pump, 1650L ammoniacal liquor is squeezed into DPG material-compound tank, pours DPG reactor into by dnockout pump simultaneously;
Feed intake complete, stop material-compound tank immediately and stir, close section door;
(2) DPG oxidation
To check on reactor section door switch determine errorless after, start and stir, slowly pass into steam to chuck, control at 26 minutes, make still temperature reach 56 DEG C, stop heating;
First open the total section door entering under meter from oxygen-supplying tube; slowly section door imported and exported by turn-on flow rate meter; regulate logical oxygen speed; oxygen section door is entered under opening the liquid on DPG reactor again; concrete control is: 28Kg/h in earlier stage; later stage falls after rise naturally, until be difficult to into oxygen under 0.32MPa pressure, complete by the fixed qualified rear reaction of middle detection;
When still pressure stabilizes to 0.32MPa, oxidation flow falls after rise naturally, illustrates that reaction may be reached home, timely sampling analysis; confirm to arrive terminal, namely stop logical oxygen, do not arrive terminal, slowly oxygenating; repeat to judge, continue sampling analysis, until DPG content till 98.5%;
(3) DPG washing, drying
Check DPG water washing tank, close water washing tank emptying section door, close DPG water washing tank washing section door, open DPG water washing tank to DPG mother liquor tank section door;
Slowly open oxidation tank discharging section door, while stirring material is all put into water washing tank;
Open air compressor machine, on cleaning of evaporator of fetching boiling water, compressed air body segment door, is depressed into DPG mother liquor tank by mother liquor, volume 2200L, as first pass mother liquor;
After oxidation tank has gone out material; 800L water is added in tank; put into the water washing tank of having pressed mother liquor while stirring; add again after 300L washes oxidation tank and put into DPG water washing tank, then open stirring 5 minutes, close after stirring; open compression section door; mother liquor is pressed into DPG mother liquor tank, volume 1000L, as second time mother liquor;
Add 1500L water to DPG water washing tank, open water cleaning of evaporator stirs 5 minutes, after stirring, and closes and stirs, and opens compression section door, mother liquor is depressed into DPG mother liquor tank, runs empty after volume 1400L;
Close DPG mother liquor tank to DPG water washing tank section door, open DPG water washing tank washing section door, add washing material;
Add half tank water again, release material while stirring and dry, get rid of to drier outlet without water droplet;
(4) dry, sieve, pack
Monitoring device pipeline, opens induced draft fan, opens heater steam, steam regulation pressure, make inlet temperature be 127 DEG C;
Fed in raw material by the guard of feeder, control dry temperature out 52 DEG C with feed rate;
Open forward and backward storehouse air sealer and automatic sieving machine and vibrator, after taking out material, can product be obtained.
Usefulness of the present invention is: the method can improve productive rate and the purity of vulkacit D PG, improves output and quality product, reduces production cost, and the rubber product foreign matter content that the promotor that this method of use is made is produced is low, prolongation in work-ing life.
(4) embodiment
Embodiment 1
A production technique of rubber accelerator DPG, is characterized in that:
Concrete steps are as follows:
(1) DPG synthesis:
1. prepare burden
Check whether DPG reactor possesses formal driving condition, and perform the button-up operations fed intake;
Close material-compound tank discharging section door, open the emptying section door of material-compound tank, open vulkacit D PTU feeding cover, drop into 450kg vulkacit D PTU and 500g catalyzer to material-compound tank, finish and namely cover tightly charging opening;
Unlatching joins ammonia pump to the corresponding section door of DPG material-compound tank, starts to squeeze into into aqua ammonia pump to DPG material-compound tank surely to throw ammonia vol 1650L by middle detection;
Start material-compound tank to stir, after evenly. open emptying section door on material-compound tank bottom discharge section door and corresponding DPG reactor, open corresponding section door and corresponding DPG oxidation tank upper feeding section door on material-compound tank dnockout pipeline, start dnockout pump to DPG reactor feed;
Treat that in material-compound tank, material is beaten to the greatest extent, then open into aqua ammonia pump, 1650L ammoniacal liquor is squeezed into DPG material-compound tank, pours DPG reactor into by dnockout pump simultaneously;
Feed intake complete, stop material-compound tank immediately and stir, close section door;
(2) DPG oxidation
To check on reactor section door switch determine errorless after, start and stir, slowly pass into steam to chuck, control at 26 minutes, make still temperature reach 56 DEG C, stop heating;
First open the total section door entering under meter from oxygen-supplying tube; slowly section door imported and exported by turn-on flow rate meter; regulate logical oxygen speed; oxygen section door is entered under opening the liquid on DPG reactor again; concrete control is: 28Kg/h in earlier stage; later stage falls after rise naturally, until be difficult to into oxygen under 0.32MPa pressure, complete by the fixed qualified rear reaction of middle detection;
When still pressure stabilizes to 0.32MPa, oxidation flow falls after rise naturally, illustrates that reaction may be reached home, timely sampling analysis; confirm to arrive terminal, namely stop logical oxygen, do not arrive terminal, slowly oxygenating; repeat to judge, continue sampling analysis, until DPG content till 98.5%;
(3) DPG washing, drying
Check DPG water washing tank, close water washing tank emptying section door, close DPG water washing tank washing section door, open DPG water washing tank to DPG mother liquor tank section door;
Slowly open oxidation tank discharging section door, while stirring material is all put into water washing tank;
Open air compressor machine, on cleaning of evaporator of fetching boiling water, compressed air body segment door, is depressed into DPG mother liquor tank by mother liquor, volume 2200L, as first pass mother liquor;
After oxidation tank has gone out material; 800L water is added in tank; put into the water washing tank of having pressed mother liquor while stirring; add again after 300L washes oxidation tank and put into DPG water washing tank, then open stirring 5 minutes, close after stirring; open compression section door; mother liquor is pressed into DPG mother liquor tank, volume 1000L, as second time mother liquor;
Add 1500L water to DPG water washing tank, open water cleaning of evaporator stirs 5 minutes, after stirring, and closes and stirs, and opens compression section door, mother liquor is depressed into DPG mother liquor tank, runs empty after volume 1400L;
Close DPG mother liquor tank to DPG water washing tank section door, open DPG water washing tank washing section door, add washing material;
Add half tank water again, release material while stirring and dry, get rid of to drier outlet without water droplet;
(4) dry, sieve, pack
Monitoring device pipeline, opens induced draft fan, opens heater steam, steam regulation pressure, make inlet temperature be 127 DEG C;
Fed in raw material by the guard of feeder, control dry temperature out 52 DEG C with feed rate;
Open forward and backward storehouse air sealer and automatic sieving machine and vibrator, after taking out material, can product be obtained.
As calculated, the vulkacit D PG productive rate 98% that this law is obtained, purity 99%.
Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.

Claims (2)

1. a production technique of rubber accelerator DPG, is characterized in that:
Concrete steps are as follows:
(1) DPG synthesis:
1. prepare burden
Check whether DPG reactor possesses formal driving condition, and perform the button-up operations fed intake;
Close material-compound tank discharging section door, open the emptying section door of material-compound tank, open vulkacit D PTU feeding cover, drop into 450kg vulkacit D PTU and 500g catalyzer to material-compound tank, finish and namely cover tightly charging opening;
Unlatching joins ammonia pump to the corresponding section door of DPG material-compound tank, starts to squeeze into into aqua ammonia pump to DPG material-compound tank surely to throw ammonia vol 1650L by middle detection;
Start material-compound tank to stir, after evenly. open emptying section door on material-compound tank bottom discharge section door and corresponding DPG reactor, open corresponding section door and corresponding DPG oxidation tank upper feeding section door on material-compound tank dnockout pipeline, start dnockout pump to DPG reactor feed;
Treat that in material-compound tank, material is beaten to the greatest extent, then open into aqua ammonia pump, 1650L ammoniacal liquor is squeezed into DPG material-compound tank, pours DPG reactor into by dnockout pump simultaneously;
Feed intake complete, stop material-compound tank immediately and stir, close section door;
(2) DPG oxidation
To check on reactor section door switch determine errorless after, start and stir, slowly pass into steam to chuck, control at 25 ~ 30 minutes, make still temperature reach 56 DEG C, stop heating;
First open the total section door entering under meter from oxygen-supplying tube; slowly section door imported and exported by turn-on flow rate meter; regulate logical oxygen speed; oxygen section door is entered under opening the liquid on DPG reactor again; concrete control is: in earlier stage≤30Kg/h; later stage falls after rise naturally, until be difficult to into oxygen under 0.32MPa pressure, complete by the fixed qualified rear reaction of middle detection;
When still pressure stabilizes to 0.32MPa, oxidation flow falls after rise naturally, illustrates that reaction may be reached home, timely sampling analysis; confirm to arrive terminal, namely stop logical oxygen, do not arrive terminal, slowly oxygenating; repeat to judge, continue sampling analysis, until DPG content till 98.5%;
(3) DPG washing, drying
Check DPG water washing tank, close water washing tank emptying section door, close DPG water washing tank washing section door, open DPG water washing tank to DPG mother liquor tank section door;
Slowly open oxidation tank discharging section door, while stirring material is all put into water washing tank;
Open air compressor machine, on cleaning of evaporator of fetching boiling water, compressed air body segment door, is depressed into DPG mother liquor tank by mother liquor, volume 2200L, as first pass mother liquor;
After oxidation tank has gone out material; 800L water is added in tank; put into the water washing tank of having pressed mother liquor while stirring; add again after 300L washes oxidation tank and put into DPG water washing tank, then open stirring 5 minutes, close after stirring; open compression section door; mother liquor is pressed into DPG mother liquor tank, volume 1000 liters, as second time mother liquor;
Add 1500L water to DPG water washing tank, open water cleaning of evaporator stirs 5 minutes, after stirring, and closes and stirs, and opens compression section door, mother liquor is depressed into DPG mother liquor tank, runs empty after volume 1400L;
Close DPG mother liquor tank to DPG water washing tank section door, open DPG water washing tank washing section door, add washing material;
Add water again, release material while stirring and dry, get rid of to drier outlet without water droplet;
(4) dry, sieve, pack
Monitoring device pipeline, opens induced draft fan, opens heater steam, steam regulation pressure, make inlet temperature be 110-135 DEG C;
Fed in raw material by the guard of feeder, control dry temperature out 45 ~ 55 DEG C with feed rate;
Open forward and backward storehouse air sealer and automatic sieving machine and vibrator, after taking out material, can product be obtained.
2. the production technique of a kind of rubber accelerator DPG according to claim 1, is characterized in that:
Concrete steps are as follows:
(1) DPG synthesis:
1. prepare burden
Check whether DPG reactor possesses formal driving condition, and perform the button-up operations fed intake;
Close material-compound tank discharging section door, open the emptying section door of material-compound tank, open vulkacit D PTU feeding cover, drop into 450kg vulkacit D PTU and 500g catalyzer to material-compound tank, finish and namely cover tightly charging opening;
Unlatching joins ammonia pump to the corresponding section door of DPG material-compound tank, starts to squeeze into into aqua ammonia pump to DPG material-compound tank surely to throw ammonia vol 1650L by middle detection;
Start material-compound tank to stir, after evenly. open emptying section door on material-compound tank bottom discharge section door and corresponding DPG reactor, open corresponding section door and corresponding DPG oxidation tank upper feeding section door on material-compound tank dnockout pipeline, start dnockout pump to DPG reactor feed;
Treat that in material-compound tank, material is beaten to the greatest extent, then open into aqua ammonia pump, 1650L ammoniacal liquor is squeezed into DPG material-compound tank, pours DPG reactor into by dnockout pump simultaneously;
Feed intake complete, stop material-compound tank immediately and stir, close section door;
(2) DPG oxidation
To check on reactor section door switch determine errorless after, start and stir, slowly pass into steam to chuck, control at 26 minutes, make still temperature reach 56 DEG C, stop heating;
First open the total section door entering under meter from oxygen-supplying tube; slowly section door imported and exported by turn-on flow rate meter; regulate logical oxygen speed; oxygen section door is entered under opening the liquid on DPG reactor again; concrete control is: 28Kg/h in earlier stage; later stage falls after rise naturally, until be difficult to into oxygen under 0.32MPa pressure, complete by the fixed qualified rear reaction of middle detection;
When still pressure stabilizes to 0.32MPa, oxidation flow falls after rise naturally, illustrates that reaction may be reached home, timely sampling analysis; confirm to arrive terminal, namely stop logical oxygen, do not arrive terminal, slowly oxygenating; repeat to judge, continue sampling analysis, until DPG content till 98.5%;
(3) DPG washing, drying
Check DPG water washing tank, close water washing tank emptying section door, close DPG water washing tank washing section door, open DPG water washing tank to DPG mother liquor tank section door;
Slowly open oxidation tank discharging section door, while stirring material is all put into water washing tank;
Open air compressor machine, on cleaning of evaporator of fetching boiling water, compressed air body segment door, is depressed into DPG mother liquor tank by mother liquor, volume 2200L, as first pass mother liquor;
After oxidation tank has gone out material; 800L water is added in tank; put into the water washing tank of having pressed mother liquor while stirring; add again after 300L washes oxidation tank and put into DPG water washing tank, then open stirring 5 minutes, close after stirring; open compression section door; mother liquor is pressed into DPG mother liquor tank, volume 1000L, as second time mother liquor;
Add 1500L water to DPG water washing tank, open water cleaning of evaporator stirs 5 minutes, after stirring, and closes and stirs, and opens compression section door, mother liquor is depressed into DPG mother liquor tank, runs empty after volume 1400L;
Close DPG mother liquor tank to DPG water washing tank section door, open DPG water washing tank washing section door, add washing material;
Add half tank water again, release material while stirring and dry, get rid of to drier outlet without water droplet;
(4) dry, sieve, pack
Monitoring device pipeline, opens induced draft fan, opens heater steam, steam regulation pressure, make inlet temperature be 127 DEG C;
Fed in raw material by the guard of feeder, control dry temperature out 52 DEG C with feed rate;
Open forward and backward storehouse air sealer and automatic sieving machine and vibrator, after taking out material, can product be obtained.
CN201310643889.0A 2013-12-03 2013-12-03 Production process of rubber accelerator DPG Pending CN104672109A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106631907A (en) * 2016-10-14 2017-05-10 山东尚舜化工有限公司 Synthetic rubber accelerator system and technique
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106631907A (en) * 2016-10-14 2017-05-10 山东尚舜化工有限公司 Synthetic rubber accelerator system and technique
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

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Application publication date: 20150603