CN105296004B - Processing technology for chlorinated paraffin - Google Patents
Processing technology for chlorinated paraffin Download PDFInfo
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- CN105296004B CN105296004B CN201510615260.4A CN201510615260A CN105296004B CN 105296004 B CN105296004 B CN 105296004B CN 201510615260 A CN201510615260 A CN 201510615260A CN 105296004 B CN105296004 B CN 105296004B
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Abstract
The invention relates to a processing technology for chlorinated paraffin. A chlorinated paraffin product is obtained by using wax oil and chlorine as raw materials and adopting a seven-stage continuous photo-thermal catalytic chlorination process and a bubbling degassing technology. The processing technology for the chlorinated paraffin, which is disclosed by the invention, comprises the following steps of: liquid chlorine gasification, chlorination and chlorinated tail gas adsorption. The processing technology which is disclosed by the invention is simple, is short in reaction time, and is high in conversion rate; production cost is reduced; economic benefits of enterprises are increased.
Description
Technical field
The present invention relates to a kind of preparation method of auxiliary agent, specifically a kind of processing technique of chlorinated paraffin.
Background technology
Chlorinated paraffin is the chlorinated derivatives of paraffin hydrocarbon, has low volatility, fire-retardant, electrical insulating property is good, inexpensive etc. excellent
Point, be widely used in production CABLE MATERIALS, the product such as plate, flexible pipe, artificial leather, rubber.At present, domestic production technology of chlorinated paraffin
Mainly there are 3 kinds: thermal chlorination, catalysis method, photocatalytic method, but every kind of method could obtain after being required for multiple step reaction
To chlorinated paraffin finished product, response time length, high cost, and complex process.
Content of the invention
In order to solve the above problems, the invention provides a kind of is raw material using wax oil and chlorine, by 7 grades of continuous photo-thermal
Catalytic chlorination technique, bubbling Degassing Technology obtains the processing technique of chlorinated paraffin product.
In order to achieve the above object, the present invention is achieved by the following technical solutions:
The present invention is a kind of processing technique of chlorinated paraffin, and described processing technique comprises the steps:
(1) liquid chlorine vaporizing: open liquid chlorine gasifier inlet valve, add water to full liquid level, open steam heating water, control water
Not higher than 45 DEG C of temperature, opens liquid chlorine tank car liquid outlet valve, liquid chlorine is passed through liquid chlorine gasifier and is gasified, and gasification chlorine enters
Chlorine Buffer Vessel, control Chlorine Buffer Vessel pressure is 0.35mpa, and in surge tank, chlorine uses for chloridizing unit；
(2) chlorination reaction: from the raw material wax oil of tank area, squeeze into workshop wax oil measuring tank through wax oil discharging pump, then warp
Workshop wax oil pump is squeezed into three-level and is checked on kettle, and three-level kettle of checking on is flow to two grades and checks on from three-level kettle of checking on successively using the liquid level discrepancy in elevation
The concentrated hydrochloric acid that kettle, one-level are checked in kettle and the net scrubbing tower of extraction, with the net scrubbing tower of extraction carries out intersecting mixing, micro- in extraction wax oil
Amount hydrochloric acid；Net scrubbing tower is suitable for reading to be flowed in the first chlorination tank by extracting to extract wax oil in net scrubbing tower, opens workshop wax oil measuring tank
Discharging pump, wax oil enters three-level through effusion meter and checks on kettle, flows into the first chlorination tank using the liquid level discrepancy in elevation, wax oil is from the first chlorination tank
Flow into the second chlorination tank, then flow into tri-chlorination kettle from the second chlorination tank, then flow into the 4th chlorination tank from tri-chlorination kettle, then from
4th chlorination tank flows into phosphoric kettle, then flows into the 6th chlorination tank from phosphoric kettle, then flows into the 7th from the 6th chlorination tank
Chlorination tank, the 7th chlorination tank chlorinated paraffin enters chlorinated paraffin receiving slit；
Open chlorine feed valve, control the first chlorination tank chlorine flowrate, the second chlorination tank chlorine flowrate, tri-chlorination kettle
Chlorine flowrate, the 4th chlorination tank chlorine flowrate, phosphoric kettle chlorine flowrate, the 6th chlorination tank chlorine flowrate, the 7th chlorination tank
Chlorine flowrate, routine test tri-chlorination kettle, phosphoric kettle, the 7th chlorination tank chlorine density simultaneously, control density 1.21 ~
1.23g/ml, according to the logical chlorine dose of density adjustment, controls chlorination tank temperature at 95 DEG C ~ 110 DEG C, when more than 110 DEG C, turns down chlorine
Inlet amount, and reduce wax oil inlet amount simultaneously, adjust cooling water circulation amount simultaneously；
After in production process, the chlorine of the hydrogen chloride gas of generation and undone reaction separates through the first cyclone separator, liquid
Body enters the 7th chlorination tank, and gas removes one-level graphite film-falling absorption tower absorbing hydrogen chloride gas, and one-level graphite film-falling absorption tower is out
Gas enter one-level and check on and absorb chlorine in kettle, one-level is checked on after kettle gas out separates through the second cyclone separator and is entered
Two grades of graphite film-falling absorption tower absorbing hydrogen chloride gases, two grades of graphite film-falling absorption towers gas out enters two by ejector pump
Level kettle of checking on absorbs chlorine, and two grades of kettle gases out of checking on enter one-level packed absorber absorbing hydrogen chloride gases, and one-level is filled out
Material absorption tower gas out enters three-level kettle of checking on by ejector pump and absorbs chlorine, and three-level kettle gas out of checking on passes through to spray
Penetrate pump and enter dilute acid bath absorbing hydrogen chloride gas, dilute acid bath gas out enters two grades of packed tower absorbing hydrogen chloride gases, and
Two grades of packed towers gas out will be vented；
Open discharge pump, the chlorinated paraffin in chlorinated paraffin receiving slit is squeezed into degassing kettle, add stable after about 90 minutes
Agent, finished product chlorinated paraffin, degassing kettle gas out, through degassing tempering tower, enters three-level packed tower and absorbs, finished product chlorine
Fossil waxes squeeze into finished product storage tank through discharge pump.
Further improvement of the present invention is: the hydrogen chloride tail gas of the present invention absorb and are broadly divided into two sets of different techniques:
The hydrogen chloride tail gas producing in chlorinated paraffin production process absorb through one-level graphite film-falling absorption tower, two grades of graphite falls
Film absorption tower absorbs, one-level packed tower absorbs, two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, by-product
Hydrochloric acid squeezes into hydrochloric acid tank through concentrated hydrochloric acid pump；
Or the hydrogen chloride gas producing and unreacted chlorine divide through the second cyclone separator in chlorinated paraffin production process
From after remove one-level sink, after washing, liquid removes the first chlorination tank, and tail gas removes two grades of sinks, the scrubbed pump of the liquid after washing
Beat to one-level scrubbing tower, tail gas absorbs through one-level graphite film-falling absorption tower, two grades of absorptions of graphite film-falling absorption tower, one-level packed towers
Absorb, two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, by-product hydrochloric acid part squeezes into salt through concentrated hydrochloric acid pump
Acid storage tank.
The invention has the beneficial effects as follows: the chlorinated paraffin that the present invention provides only needs an one-step chlorination reaction to obtain finished product, its
Reaction principle is as follows: reaction equation:, with wax oil and chlorine as raw material, adopt 7
The continuous photo-thermal catalytic chlorination technique of level, bubbling Degassing Technology, obtain chlorinated paraffin product, preparation process includes liquid chlorine vaporizing, chlorine
Change reaction and chlorinated exhaust absorbs, the production of chlorinated paraffin employs national at present more advanced continuous production processes, adopts 7
Individual chlorination tank is cascaded, and using the principle of liquid level differential pressure, raw material paraffin oil flows to the second chlorination tank from the first chlorination tank,
Until flowing to the 7th chlorination tank, and the 7th chlorination tank is finished product chlorinated paraffin；7 chlorination tanks all lead to the chlorine of different flow,
Reacted with the paraffin oil in chlorination tank, until the paraffin oil in the 7th chlorination tank reaches the quality standard of product, finished product chlorine
The discharge method of fossil waxes becomes seriality discharging；The absorption of chlorinated exhaust is also the domestic more advanced absorption adopting at present
Principle, referred to as three-level are checked on, Pyatyi absorbs, and three-level is checked on as tri- enamel reaction stills of 3m, 4m, 6m, primarily serves absorption chlorine
Change the chlorine of not reaction completely in tail gas, accomplish chlorine qualified discharge；Pyatyi be absorbed as two graphite falling film absorption and three fill out
Material absorbs, and absorbent is tap water, to absorb the hydrogen chloride gas that chlorination reaction goes out, and makes technical hydrochloric acid, accomplishes hydrogen chloride gas
Body qualified discharge.The discharge method of hydrochloric acid becomes seriality discharging.
The processing technique of the present invention is simple, and the response time is short, high conversion rate, reduces production cost, improves enterprise
Economic benefit.
Brief description
Fig. 1 is the process chart of the present invention.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with drawings and Examples, the present invention is done and retouch in detail further
State, this embodiment is only used for explaining the present invention, protection scope of the present invention is not constituted and limits.
As shown in Fig. 1, the present invention is a kind of processing technique of chlorinated paraffin, and described processing technique comprises the steps:
(1) liquid chlorine vaporizing: open liquid chlorine gasifier inlet valve, add water to full liquid level, open steam heating water, control water
Not higher than 45 DEG C of temperature, opens liquid chlorine tank car liquid outlet valve, liquid chlorine is passed through liquid chlorine gasifier, that is, coil pipe gasifier is carried out
Gasification, gasification chlorine enters Chlorine Buffer Vessel, and control Chlorine Buffer Vessel pressure is 0.35mpa, and in surge tank, chlorine supplies chlorination to fill
Put use；
(2) chlorination reaction: from the raw material wax oil of tank area, squeeze into workshop wax oil measuring tank through wax oil discharging pump, then warp
Workshop wax oil pump is squeezed into three-level and is checked on kettle, and three-level kettle of checking on is flow to two grades and checks on from three-level kettle of checking on successively using the liquid level discrepancy in elevation
The concentrated hydrochloric acid that kettle, one-level are checked in kettle and the net scrubbing tower of extraction, with the net scrubbing tower of extraction carries out intersecting mixing, micro- in extraction wax oil
Amount hydrochloric acid；Net scrubbing tower is suitable for reading to be flowed in the first chlorination tank by extracting to extract wax oil in net scrubbing tower, opens workshop wax oil measuring tank
Discharging pump, wax oil enters three-level through effusion meter and checks on kettle, flows into the first chlorination tank using the liquid level discrepancy in elevation, wax oil is from the first chlorination tank
Flow into the second chlorination tank, then flow into tri-chlorination kettle from the second chlorination tank, then flow into the 4th chlorination tank from tri-chlorination kettle, then from
4th chlorination tank flows into phosphoric kettle, then flows into the 6th chlorination tank from phosphoric kettle, then flows into the 7th from the 6th chlorination tank
Chlorination tank, the 7th chlorination tank chlorinated paraffin enters chlorinated paraffin receiving slit；
Open chlorine feed valve, control the first chlorination tank chlorine flowrate, the second chlorination tank chlorine flowrate, tri-chlorination kettle
Chlorine flowrate, the 4th chlorination tank chlorine flowrate, phosphoric kettle chlorine flowrate, the 6th chlorination tank chlorine flowrate, the 7th chlorination tank
Chlorine flowrate, routine test tri-chlorination kettle, phosphoric kettle, the 7th chlorination tank chlorine density simultaneously, control density 1.21 ~
1.23g/ml, according to the logical chlorine dose of density adjustment, controls chlorination tank temperature at 95 DEG C ~ 110 DEG C, when more than 110 DEG C, turns down chlorine
Inlet amount, and reduce wax oil inlet amount simultaneously, adjust cooling water circulation amount simultaneously；
After in production process, the chlorine of the hydrogen chloride gas of generation and undone reaction separates through the first cyclone separator, liquid
Body enters the 7th chlorination tank, and gas removes one-level graphite film-falling absorption tower absorbing hydrogen chloride gas, and one-level graphite film-falling absorption tower is out
Gas enter one-level and check on and absorb chlorine in kettle, one-level is checked on after kettle gas out separates through the second cyclone separator and is entered
Two grades of graphite film-falling absorption tower absorbing hydrogen chloride gases, two grades of graphite film-falling absorption towers gas out enters two by ejector pump
Level kettle of checking on absorbs chlorine, and two grades of kettle gases out of checking on enter one-level packed absorber absorbing hydrogen chloride gases, and one-level is filled out
Material absorption tower gas out enters three-level kettle of checking on by ejector pump and absorbs chlorine, and three-level kettle gas out of checking on passes through to spray
Penetrate pump and enter dilute acid bath absorbing hydrogen chloride gas, dilute acid bath gas out enters two grades of packed tower absorbing hydrogen chloride gases, and
Two grades of packed towers gas out will be vented；
Open discharge pump, the chlorinated paraffin in chlorinated paraffin receiving slit is squeezed into degassing kettle, degassing kettle can for two simultaneously
The degassing kettle of row setting is carried out simultaneously, adds stabilizer, finished product chlorinated paraffin after about 90 minutes, and deaerate kettle gas out
Through the tempering tower that deaerates, enter three-level packed tower and absorb, finished product chlorinated paraffin squeezes into finished product storage tank through discharge pump.
In chlorinated paraffin machining process of the present invention, hydrogen chloride tail gas absorb and are divided into two sets of different devices, specifically such as
Under:
The hydrogen chloride tail gas producing in chlorinated paraffin production process absorb through one-level graphite film-falling absorption tower, two grades of graphite falls
Film absorption tower absorbs, one-level packed tower absorbs, two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, by-product
Hydrochloric acid squeezes into hydrochloric acid tank through concentrated hydrochloric acid pump；
Or the hydrogen chloride gas producing and unreacted chlorine divide through the second cyclone separator in chlorinated paraffin production process
From after remove one-level sink, after washing, liquid removes the first chlorination tank, and tail gas removes two grades of sinks, the scrubbed pump of the liquid after washing
Beat to one-level scrubbing tower, tail gas absorbs through one-level graphite film-falling absorption tower, two grades of absorptions of graphite film-falling absorption tower, one-level packed towers
Absorb, two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, by-product hydrochloric acid part squeezes into salt through concentrated hydrochloric acid pump
Acid storage tank.
Claims (2)
1. a kind of processing technique of chlorinated paraffin it is characterised in that: described processing technique comprises the steps:
(1) liquid chlorine vaporizing: open liquid chlorine gasifier inlet valve, add water to full liquid level, open steam heating water, control water temperature not
Higher than 45 DEG C, open liquid chlorine tank car liquid outlet valve, liquid chlorine is passed through liquid chlorine gasifier and is gasified, gasification chlorine enters chlorine
Surge tank, control Chlorine Buffer Vessel pressure is 0.35mpa, and in surge tank, chlorine uses for chloridizing unit；
(2) chlorination reaction: from the raw material wax oil of tank area, squeeze into workshop wax oil measuring tank through wax oil discharging pump, then through workshop
Wax oil pump is squeezed into three-level and is checked on kettle, three-level check on kettle using the liquid level discrepancy in elevation successively from three-level check on kettle flow to two grades of kettles of checking on, one
The concentrated hydrochloric acid that level is checked in kettle and the net scrubbing tower of extraction, with the net scrubbing tower of extraction carries out intersecting mixing, the trace salt in extraction wax oil
Acid；Net scrubbing tower is suitable for reading to be flowed in the first chlorination tank by extracting to extract wax oil in net scrubbing tower, opens workshop wax oil measuring tank discharging
Pump, wax oil enters three-level through effusion meter and checks on kettle, flows into the first chlorination tank using the liquid level discrepancy in elevation, and wax oil flows into from the first chlorination tank
Second chlorination tank, then flow into tri-chlorination kettle from the second chlorination tank, then flow into the 4th chlorination tank from tri-chlorination kettle, then from the 4th
Chlorination tank flows into phosphoric kettle, then flows into the 6th chlorination tank from phosphoric kettle, then flows into heptachlor from the 6th chlorination tank
Kettle, the 7th chlorination tank chlorinated paraffin enters chlorinated paraffin receiving slit；
Open chlorine feed valve, control the first chlorination tank chlorine flowrate, the second chlorination tank chlorine flowrate, tri-chlorination kettle chlorine
Flow, the 4th chlorination tank chlorine flowrate, phosphoric kettle chlorine flowrate, the 6th chlorination tank chlorine flowrate, the 7th chlorination tank chlorine
Flow, routine test tri-chlorination kettle, phosphoric kettle, the 7th chlorination tank chlorine density simultaneously, control density 1.21 ~
1.23g/ml, according to the logical chlorine dose of density adjustment, controls chlorination tank temperature at 95 DEG C ~ 110 DEG C, when more than 110 DEG C, turns down chlorine
Inlet amount, and reduce wax oil inlet amount simultaneously, adjust cooling water circulation amount simultaneously；
, after the first cyclone separator separation, liquid enters for the hydrogen chloride gas producing in production process and the chlorine of undone reaction
7th chlorination tank, gas removes one-level graphite film-falling absorption tower absorbing hydrogen chloride gas, one-level graphite film-falling absorption tower gas out
Body entrance one-level is checked on, and kettle is interior to absorb chlorine, and one-level is checked on after kettle gas out separates through the second cyclone separator and entered two grades
Graphite film-falling absorption tower absorbing hydrogen chloride gas, two grades of graphite film-falling absorption towers gas out enters two grades of handles by ejector pump
Close kettle and absorb chlorine, two grades of kettle gases out of checking on enter one-level packed absorber absorbing hydrogen chloride gas, and one-level filler is inhaled
Receive tower gas out three-level kettle of checking on is entered by ejector pump and absorb chlorine, three-level checks on kettle gas out by ejector pump
Enter dilute acid bath absorbing hydrogen chloride gas, dilute acid bath gas out enters two grades of packed tower absorbing hydrogen chloride gases, and two grades
Packed tower gas out will be vented；
Open discharge pump, the chlorinated paraffin in chlorinated paraffin receiving slit is squeezed into degassing kettle, after about 90 minutes, add stabilizer, system
Obtain finished product chlorinated paraffin, degassing kettle gas out, through degassing tempering tower, enters the absorption of three-level packed tower, finished product chlorinated paraffin
Squeeze into finished product storage tank through discharge pump.
2. according to claim 1 a kind of processing technique of chlorinated paraffin it is characterised in that: in chlorinated paraffin production process produce
Raw hydrogen chloride tail gas absorb through one-level graphite film-falling absorption tower, two grades of graphite film-falling absorption towers absorb, one-level packed tower absorbs,
Two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, and by-product hydrochloric acid squeezes into hydrochloric acid tank through concentrated hydrochloric acid pump；
Or in chlorinated paraffin production process produce hydrogen chloride gas and unreacted chlorine through second cyclone separator separate after
Remove one-level sink, after washing, liquid removes the first chlorination tank, tail gas removes two grades of sinks, the scrubbed pump of the liquid after washing beat to
One-level scrubbing tower, tail gas absorbs through one-level graphite film-falling absorption tower, two grades of absorptions of graphite film-falling absorption tower, one-level packed towers are inhaled
Receive, two grades of packed tower absorptions, three-level packed towers absorb and obtain byproduct hydrochloric acid, by-product hydrochloric acid part squeezes into hydrochloric acid through concentrated hydrochloric acid pump
Storage tank.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615260.4A CN105296004B (en) | 2015-09-18 | 2015-09-18 | Processing technology for chlorinated paraffin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615260.4A CN105296004B (en) | 2015-09-18 | 2015-09-18 | Processing technology for chlorinated paraffin |
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| CN105296004A CN105296004A (en) | 2016-02-03 |
| CN105296004B true CN105296004B (en) | 2017-02-01 |
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| CN106362555B (en) * | 2016-09-12 | 2019-06-28 | 江苏九九久科技有限公司 | Process gas purifying treatment method |
| CN107142124B (en) * | 2017-06-26 | 2019-03-12 | 柳州市隆达丰化工科技有限公司 | A kind of method that thermal chlorination produces chlorinated paraffin -52 in conjunction with photocatalytic method |
| CN108034454A (en) * | 2017-12-12 | 2018-05-15 | 宁波镇洋化工发展有限公司 | A kind of chlorinated-paraffin producing process |
| CN108315054A (en) * | 2018-02-12 | 2018-07-24 | 丹阳市助剂化工厂有限公司 | Chlorinated paraffin continuous production processes |
| CN108201739B (en) * | 2018-02-12 | 2024-01-02 | 丹阳市助剂化工厂有限公司 | Chlorinated paraffin raw material pretreatment equipment |
| CN108159786B (en) * | 2018-02-12 | 2024-01-30 | 丹阳市助剂化工厂有限公司 | Chlorinated paraffin tail gas pretreatment equipment |
| CN109022035A (en) * | 2018-08-15 | 2018-12-18 | 安徽绿色谷创客空间股份有限公司 | A kind of efficient process units and production method of chlorinated paraffin |
| CN110420611A (en) * | 2019-09-06 | 2019-11-08 | 丹阳市助剂化工厂有限公司 | A kind of chlorination tank producing chlorinated paraffin |
| CN110523226A (en) * | 2019-09-09 | 2019-12-03 | 丹阳市助剂化工厂有限公司 | A kind of Chlorcosane tail gas treatment process and absorption equipment |
| CN110422825A (en) * | 2019-09-09 | 2019-11-08 | 丹阳市助剂化工厂有限公司 | A kind of HCl recovery Processes and apparatus in chlorinated paraffin production process |
| CN111589292A (en) * | 2020-05-28 | 2020-08-28 | 山东振曦新材料科技有限公司 | Non-alkalization treatment process for tail gas of methyl chloride fatty acid |
| CN111589293A (en) * | 2020-05-28 | 2020-08-28 | 山东振曦新材料科技有限公司 | Chlorinated fatty acid methyl ester tail gas non-alkalization treatment system |
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| CN103160321A (en) * | 2013-04-01 | 2013-06-19 | 南京国威化工有限公司 | Method and equipment for continuously refining liquid paraffin by virtue of by-product hydrochloric acid during chlorinated paraffin production |
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| US6114591A (en) * | 1994-11-09 | 2000-09-05 | Dover Chemical Corporation | Process for preparing highly chlorinated paraffins |
| CN101544911A (en) * | 2009-05-06 | 2009-09-30 | 河南省化工研究所有限责任公司 | Self circulation heat exchange method for materials in production of chlorinating paraffin-52 and chlorination reaction device therefor |
| CN103160321A (en) * | 2013-04-01 | 2013-06-19 | 南京国威化工有限公司 | Method and equipment for continuously refining liquid paraffin by virtue of by-product hydrochloric acid during chlorinated paraffin production |
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