CN110066234A - A kind of DCP reduction reaction process - Google Patents
A kind of DCP reduction reaction process Download PDFInfo
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- CN110066234A CN110066234A CN201910257937.XA CN201910257937A CN110066234A CN 110066234 A CN110066234 A CN 110066234A CN 201910257937 A CN201910257937 A CN 201910257937A CN 110066234 A CN110066234 A CN 110066234A
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- reduction
- water
- kettle
- benzylalcohol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
Abstract
The invention discloses a kind of DCP reduction reaction process, step 1: the water in the circulating water chennel of underground is prepared, reducing solution slurry as reduced sulphur choline；Step 2: preparing the vulcanization aqueous alkali needed for calculating and oxidation solution reaction in akali sulphide make-up tank, then stop stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water slot through reduction kettle discharging pump；Step 3: it is washed in kettle with the water in reduction type washing trough；Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, river adjusts control timing by flow and is layered into reduction rinsing bowl counter flow washing, grease, the oil reservoir that tower top overflows enters benzylalcohol tower feed well and settles again, thick benzylalcohol then feeds pumping rectification working process by benzylalcohol tower, which makees reducing agent using akali sulphide, has reduction reaction speed fast, the features such as benzylalcohol high income, reduction reaction is safe and reliable.
Description
Technical field
The present invention relates to DCP reduction technique field, specially a kind of DCP reduction reaction process.
Background technique
DCP, that is, dicumyl peroxide, cumyl peroxide, also known as vulcanizing agent DCP.It is a kind of strong oxidizer.It can
As the initiator of monomer polymerization, it is commonly used for vulcanizing agent, crosslinking agent, curing agent, flame-retardant additive of high molecular material etc..
That there are efficiency is lower for traditional DCP reduction reaction, and benzylalcohol yield is low, reacts the problems such as incomplete, or even cause secondary
The case where doing over again, it would therefore be highly desirable to which a kind of improved technology solves the problems, such as this in the presence of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of DCP reduction reaction processes, to solve mentioned above in the background art ask
Topic.
To achieve the above object, the invention provides the following technical scheme: a kind of DCP reduction reaction process, including following step
It is rapid:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, controls reduction reaction temperature, reaction reaches terminal
Afterwards, stop stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water slot through reduction kettle discharging pump；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
Preferably, reaction temperature is 65~70 DEG C in the step 2.
Preferably, feed rate regulating valve is arranged in reduction kettle feed inlet one end in the step 2.
Preferably, the concentration of oxidation solution is 40 ~ 55% in the step 2.
Compared with prior art, the beneficial effects of the present invention are:
(1) reducing agent is made using akali sulphide, has reduction reaction speed fast, benzylalcohol high income, reduction reaction securely and reliably waits spies
Point.
(2) by adjust inner coil pipe circulating water water, control reduction reaction temperature be 65~70 DEG C when, akali sulphide and
Oxidation solution can react completely and settle layering, and reaction efficiency highest.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of technical solution: a kind of DCP reduction reaction process, comprising the following steps:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Kettle, then will aoxidize concentration in liquid bath is 40-55% oxidation solution, passes through reduction kettle feed rate regulating valve meter through oxidation liquid pump
Amount slowly puts into the oxidation solution of formula ratio in reduction kettle, by adjusting inner coil pipe circulating water water, controls reduction reaction
Temperature is 65~70 DEG C, after reaction reaches terminal, stops stirring sedimentation layering, by the water layer containing akali sulphide, sodium sulphate through reduction kettle
Discharging pump is delivered to reducing waste water slot；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
A kind of embodiment one: DCP reduction reaction process, comprising the following steps:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, control reduction reaction temperature is 65 DEG C, reaction
Up to after terminal, stops stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water through reduction kettle discharging pump
Slot；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
When controlling reduction reaction temperature is 70 DEG C, reaction reaches maximal end point in 2 hours, then observation sedimentation, complete in sedimentation
Full response.
A kind of embodiment two: DCP reduction reaction process, comprising the following steps:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, control reduction reaction temperature is 70 DEG C, reaction
Up to after terminal, stops stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water through reduction kettle discharging pump
Slot；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
When controlling reduction reaction temperature is 65 DEG C, reaction reaches maximal end point in 2 hours, then observation sedimentation, complete in sedimentation
Full response.
A kind of embodiment three: DCP reduction reaction process, comprising the following steps:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, control reduction reaction temperature is 60 DEG C, reaction
Up to after terminal, stops stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water through reduction kettle discharging pump
Slot；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
When controlling reduction reaction temperature is 60 DEG C, reaction reaches maximal end point in 2 hours, then observation sedimentation, in sedimentation not
Reaction completely, when then to control reduction reaction temperature again be 60 DEG C, reaction reaches maximal end point in 1 hour, then observation sedimentation, sedimentation
In yet completely reaction.
A kind of example IV: DCP reduction reaction process, comprising the following steps:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, control reduction reaction temperature is 75 DEG C, reaction
Up to after terminal, stops stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water through reduction kettle discharging pump
Slot；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
When controlling reduction reaction temperature is 75 DEG C, reaction reaches maximal end point in 2 hours, then observation sedimentation, in sedimentation not
Reaction completely, when then to control reduction reaction temperature again be 75 DEG C, reaction reaches maximal end point in 1 hour, then observation sedimentation, sedimentation
In react completely.
In conclusion reaction efficiency reaches maximization when reduction reaction temperature is 65 ~ 70 DEG C.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of DCP reduction reaction process, it is characterised in that: the following steps are included:
Step 1: the water in the circulating water chennel of underground is delivered to reduction type washing trough using water-circulating pump, using as reduced sulphur choline
It prepares, reducing solution slurry；
Step 2: preparing the vulcanization aqueous alkali needed for calculating in akali sulphide make-up tank, prepare pump by vulcanized sodium and be delivered to reduction
Then kettle will aoxidize oxidation solution in liquid bath, measured by reduction kettle feed rate regulating valve by the oxygen of formula ratio through oxidation liquid pump
Change liquid slowly to put into reduction kettle, by adjusting inner coil pipe circulating water water, controls reduction reaction temperature, reaction reaches terminal
Afterwards, stop stirring sedimentation layering, the water layer containing akali sulphide, sodium sulphate is delivered to reducing waste water slot through reduction kettle discharging pump；
Step 3: it is washed in kettle with the water in reduction type washing trough, the water layer after washing and depositing is through reduction kettle discharging pump
It is delivered to reducing waste water slot, reducing solution is delivered to reduction liquid bath through reduction kettle discharging pump；
Step 4: and then reducing solution in slot is washed into feed pump through reduction, flow, which is adjusted, is sent into reduction rinsing bowl, and river is by flowing
Amount adjusts control timing and enters reduction rinsing bowl counter flow washing, grease layering, and the oil reservoir that tower top overflows enters benzylalcohol tower feed well
It settles again, reducing solution is from groove top overflow to benzylalcohol tower feed well, and the water layer to settle down is then periodically into reduction oil sump, slightly
Benzylalcohol then feeds pumping rectification working process by benzylalcohol tower.
2. a kind of DCP reduction reaction process according to claim 1, it is characterised in that: reaction temperature in the step 2
It is 65~70 DEG C.
3. a kind of DCP reduction reaction process according to claim 1, it is characterised in that: feed rate in the step 2
Regulating valve is arranged in reduction kettle feed inlet one end.
4. a kind of DCP reduction reaction process according to claim 1, it is characterised in that: oxidation solution in the step 2
Concentration is 40 ~ 55%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910257937.XA CN110066234A (en) | 2019-04-01 | 2019-04-01 | A kind of DCP reduction reaction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910257937.XA CN110066234A (en) | 2019-04-01 | 2019-04-01 | A kind of DCP reduction reaction process |
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| Publication Number | Publication Date |
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| CN110066234A true CN110066234A (en) | 2019-07-30 |
Family
ID=67366837
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| CN201910257937.XA Pending CN110066234A (en) | 2019-04-01 | 2019-04-01 | A kind of DCP reduction reaction process |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093352A (en) * | 1993-03-31 | 1994-10-12 | 兰州大学 | The manufacture method of 2-phenyl-2-propyl alcohol |
| CN203764265U (en) * | 2014-04-21 | 2014-08-13 | 太仓塑料助剂厂有限公司 | Reduction-condensation combined reaction device |
| CN104211628A (en) * | 2013-05-30 | 2014-12-17 | 中国石油化工集团公司 | Production equipment for reduction reaction for producing dicumyl peroxide and production method |
| CN107382806A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of production method of cumyl peroxide |
-
2019
- 2019-04-01 CN CN201910257937.XA patent/CN110066234A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093352A (en) * | 1993-03-31 | 1994-10-12 | 兰州大学 | The manufacture method of 2-phenyl-2-propyl alcohol |
| CN104211628A (en) * | 2013-05-30 | 2014-12-17 | 中国石油化工集团公司 | Production equipment for reduction reaction for producing dicumyl peroxide and production method |
| CN203764265U (en) * | 2014-04-21 | 2014-08-13 | 太仓塑料助剂厂有限公司 | Reduction-condensation combined reaction device |
| CN107382806A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of production method of cumyl peroxide |
Non-Patent Citations (1)
| Title |
|---|
| 刘文生 等: "硫化钠在交联剂DCP生产中引用研究", 《化学推进剂与高分子材料》 * |
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Application publication date: 20190730 |
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