CN115011378A - Production method of synthetic chlorinated paraffin - Google Patents

Production method of synthetic chlorinated paraffin Download PDF

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Publication number
CN115011378A
CN115011378A CN202110244416.8A CN202110244416A CN115011378A CN 115011378 A CN115011378 A CN 115011378A CN 202110244416 A CN202110244416 A CN 202110244416A CN 115011378 A CN115011378 A CN 115011378A
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Prior art keywords
chlorination reactor
paraffin
liquid paraffin
chlorine
chlorination
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CN202110244416.8A
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Chinese (zh)
Inventor
郭坤
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Jiangsu Guowei Chemical Co ltd
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Jiangsu Guowei Chemical Co ltd
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Priority to CN202110244416.8A priority Critical patent/CN115011378A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G73/00Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/38Chemical modification of petroleum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J10/00Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B01J10/005Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out at high temperatures in the presence of a molten material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/14Production of inert gas mixtures; Use of inert gases in general

Abstract

The invention discloses a production method of synthetic chlorinated paraffin, which comprises the following steps: s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin; s2: adding the liquid paraffin raw material in the step S2 into a chlorination reactor, filling the chlorination reactor with liquid paraffin, and heating the chlorination reactor; s3: the chlorination reactor in step S2 is communicated with an inert gas pipe, and an inert gas is injected into the chlorination reactor through the inert gas pipe. According to the invention, the chlorination reactor only comprises the liquid paraffin, the nitrogen and the chlorine, the pressure in the chlorination reactor is increased and reduced in a reciprocating manner, and the temperature in the chlorination reactor is increased and reduced in a reciprocating manner, so that the reaction of the chlorine and the liquid paraffin is accelerated, and the nitrogen is inert gas, so that the reaction of the chlorine and the liquid paraffin can be protected by the nitrogen, the full reaction of the chlorine and the liquid paraffin is effectively promoted, and the reaction rate is increased.

Description

Production method for synthesizing chlorinated paraffin
Technical Field
The invention relates to the field of chlorinated paraffin production, in particular to a production method for synthesizing chlorinated paraffin.
Background
The chlorinated paraffin is a chlorinated derivative of paraffin, has the advantages of low volatility, flame retardance, good electrical insulation, low price and the like, can be used as a flame retardant and a polyvinyl chloride auxiliary plasticizer, is widely used for producing products such as cable materials, floor materials, hoses, artificial leather, rubber and the like, is applied to additives such as polyurethane waterproof coatings, polyurethane plastic tracks, lubricating oil and the like, is suitable for flame retardance of various products, and is widely applied to the industrial fields such as plastics, rubber, fibers and the like as a plasticizer, a surface treatment agent of fabrics and packaging materials, a modifier of bonding materials and coatings, an antiwear agent for high-pressure lubrication and metal cutting processing, a mildew preventive, a waterproof agent and an ink additive.
However, in the prior art, when the chlorination reactor is in actual use, chlorine and paraffin react slowly and insufficiently, so that more chlorine tail gas exists in the chlorination reactor.
Disclosure of Invention
The invention aims to provide a production method of synthetic chlorinated paraffin, which solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the production method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material obtained in the step S2 into a chlorination reactor, filling the chlorination reactor with the liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and temperature of the chlorination reactor in the step S4, wherein the pressure changes in a range of 1-1.5Mpa in a reciprocating manner, the temperature changes in a range of 60-120 ℃ in a reciprocating manner, and starting stirring equipment in the chlorination reactor to stir the reactants;
s6: and (4) restoring the temperature of the chlorination reactor in the step (S5) to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging the chlorine gas generated in the micro reaction in the chlorination reactor for dechlorination, and finally obtaining chlorinated paraffin in the chlorination reactor.
Preferably, the temperature for heating the chlorination reactor in the step S2 is 70-80 °, and the heating time is 20 min.
Preferably, the chlorination reactor in step S2 is heated while stirring the liquid paraffin therein, and the rotation speed of the stirring device is 400-500 r/min.
Preferably, the chlorination reactor is in a sealed state in the step S2.
Preferably, the chlorine gas is injected into the chlorination reactor in the step S4, and the high-activity catalyst is injected into the chlorination reactor.
Preferably, the rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
Preferably, the stabilizing agent and the PH adjusting agent are injected into the chlorination reactor together while reducing the pressure and temperature in step S6.
Preferably, the normal temperature in step S6 is 20 °, and the normal pressure in step S6 is 0.1 MPa.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the chlorination reactor only comprises the liquid paraffin, the nitrogen and the chlorine, the pressure in the chlorination reactor is increased and reduced in a reciprocating manner, and the temperature in the chlorination reactor is increased and reduced in a reciprocating manner, so that the reaction of the chlorine and the liquid paraffin is accelerated, and the nitrogen is an inert gas, so that the nitrogen can protect the reaction of the chlorine and the liquid paraffin, and the purposes of effectively promoting the full reaction of the chlorine and the liquid paraffin and increasing the reaction rate are achieved;
2. the chlorination reactor is filled with liquid paraffin, inert gas is injected into the chlorination reactor, the liquid paraffin in the chlorination reactor is discharged outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor, and chlorine gas is injected into the chlorination reactor until the liquid paraffin occupies one third of the space of the chlorination reactor, so that the rest components in the chlorination reactor can be completely discharged, the spaces occupied by the nitrogen gas, the chlorine gas and the liquid paraffin in the chlorination reactor are the same, and the influence of other air components on the generation of the chlorinated paraffin is avoided.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that:
example one
The method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material obtained in the step S2 into a chlorination reactor, filling the chlorination reactor with the liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and the temperature of the chlorination reactor in the step S4, wherein the pressure changes in a reciprocating manner within a range of 1-1.5Mpa, the temperature changes in a reciprocating manner within a range of 60-120 ℃, and stirring the reactants by starting a stirring device in the chlorination reactor;
s6: and (4) restoring the temperature of the chlorination reactor in the step (S5) to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging the chlorine gas generated in the micro reaction in the chlorination reactor for dechlorination, and finally obtaining chlorinated paraffin in the chlorination reactor.
The heating temperature of the chlorination reactor in the step S2 is 70-80 ℃, and the heating time is 20 min.
In the step S2, the liquid paraffin in the chlorination reactor is stirred while being heated, and the rotating speed of the stirring device is 400-500 r/min.
In step S2, the chlorination reactor is sealed.
At the same time of injecting chlorine gas into the chlorination reactor in step S4, a high-activity catalyst is injected into the chlorination reactor.
The rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
The pressure and temperature are reduced in step S6 while a stabilizer and a PH adjuster are injected into the chlorination reactor together.
The normal temperature in step S6 was 20 ℃ and the normal pressure in step S6 was 0.1 MPa.
Example two
The method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material in the step S2 into a chlorination reactor, filling the chlorination reactor with liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and temperature of the chlorination reactor in the step S4, wherein the pressure changes in a range of 1-1.2Mpa in a reciprocating manner, the temperature changes in a range of 60-80 ℃ in a reciprocating manner, and starting stirring equipment in the chlorination reactor to stir the reactants;
s6: and (4) restoring the temperature of the chlorination reactor in the step (S5) to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging the chlorine gas generated in the micro reaction in the chlorination reactor for dechlorination, and finally obtaining chlorinated paraffin in the chlorination reactor.
The heating temperature of the chlorination reactor in the step S2 is 70-80 ℃, and the heating time is 20 min.
In the step S2, the liquid paraffin in the chlorination reactor is stirred while being heated, and the rotating speed of the stirring device is 400-500 r/min.
In step S2, the chlorination reactor is sealed.
At the same time of injecting chlorine gas into the chlorination reactor in step S4, a high-activity catalyst is injected into the chlorination reactor.
The rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
The stabilizer is injected into the chlorination reactor together with the PH adjuster while reducing the pressure and temperature in step S6.
The normal temperature in step S6 was 20 ℃ and the normal pressure in step S6 was 0.1 MPa.
EXAMPLE III
The method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material obtained in the step S2 into a chlorination reactor, filling the chlorination reactor with the liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and the temperature of the chlorination reactor in the step S4, wherein the pressure changes in a reciprocating manner within a range of 1.2-1.3Mpa, the temperature changes in a reciprocating manner within a range of 80-100 ℃, and stirring the reactants by starting a stirring device in the chlorination reactor;
s6: and (4) restoring the temperature of the chlorination reactor in the step (S5) to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging the chlorine gas generated in the micro reaction in the chlorination reactor for dechlorination, and finally obtaining chlorinated paraffin in the chlorination reactor.
The heating temperature of the chlorination reactor in the step S2 is 70-80 ℃, and the heating time is 20 min.
In step S2, the chlorination reactor is heated and stirs the liquid paraffin therein, and the rotation speed of the stirring device is 400-500 r/min.
In step S2, the chlorination reactor is sealed.
At the same time of chlorine gas injection into the chlorination reactor in step S4, a high-activity catalyst is injected into the chlorination reactor.
The rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
The stabilizer is injected into the chlorination reactor together with the PH adjuster while reducing the pressure and temperature in step S6.
The normal temperature in step S6 was 20 °, and the normal pressure in step S6 was 0.1 MPa.
Example four
The method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material in the step S2 into a chlorination reactor, filling the chlorination reactor with liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and the temperature of the chlorination reactor in the step S4, wherein the pressure changes in a reciprocating manner within a range of 1.3-1.5Mpa, the temperature changes in a reciprocating manner within a range of 100-120 ℃, and stirring equipment in the chlorination reactor is started to stir the reactants;
s6: and (4) restoring the temperature of the chlorination reactor in the step S5 to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging chlorine gas generated by micro reaction in the chlorination reactor, and performing dechlorination operation to obtain chlorinated paraffin in the chlorination reactor finally.
In the step S2, the heating temperature of the chlorination reactor is 70-80 ℃ and the heating time is 20 min.
In the step S2, the liquid paraffin in the chlorination reactor is stirred while being heated, and the rotating speed of the stirring device is 400-500 r/min.
In step S2, the chlorination reactor is in a sealed state.
At the same time of chlorine gas injection into the chlorination reactor in step S4, a high-activity catalyst is injected into the chlorination reactor.
The rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
The stabilizer is injected into the chlorination reactor together with the PH adjuster while reducing the pressure and temperature in step S6.
The normal temperature in step S6 was 20 °, and the normal pressure in step S6 was 0.1 MPa.
Table one:
Figure 219067DEST_PATH_IMAGE002
and (4) experimental conclusion: as can be seen from Table 1, the chlorinated paraffin prepared by the technical scheme of the invention, the liquid paraffin and the chlorine react more fully, and the chlorine content in the tail gas of the chlorination reactor is effectively reduced.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A production method of synthetic chlorinated paraffin is characterized in that: the production method comprises the following steps:
s1: preparing clean solid paraffin, and heating the solid paraffin to convert the solid paraffin into liquid paraffin;
s2: adding the liquid paraffin raw material obtained in the step S2 into a chlorination reactor, filling the chlorination reactor with the liquid paraffin, and heating the chlorination reactor;
s3: communicating the chlorination reactor in the step S2 with an inert gas pipeline, injecting inert gas into the chlorination reactor through the inert gas pipeline, and discharging liquid paraffin in the chlorination reactor outwards through a pipeline at the bottom of the chlorination reactor until the liquid paraffin occupies two thirds of the space of the chlorination reactor;
s4: the chlorination reactor in the step S3 is the same as the chlorine pipeline, and chlorine is injected into the chlorination reactor through the chlorine pipeline until the liquid paraffin occupies one third of the space of the chlorination reactor;
s5: changing the pressure and the temperature of the chlorination reactor in the step S4, wherein the pressure changes in a reciprocating manner within a range of 1-1.5Mpa, the temperature changes in a reciprocating manner within a range of 60-120 ℃, and stirring the reactants by starting a stirring device in the chlorination reactor;
s6: and (4) restoring the temperature of the chlorination reactor in the step S5 to normal temperature, restoring the pressure of the chlorination reactor to normal pressure, introducing nitrogen into the chlorination reactor, discharging chlorine gas generated by micro reaction in the chlorination reactor, and performing dechlorination operation to obtain chlorinated paraffin in the chlorination reactor finally.
2. The process for the production of the synthetic chlorinated paraffin according to claim 1, wherein: the heating temperature of the chlorination reactor in the step S2 is 70-80 degrees, and the heating time is 20 min.
3. The method for producing synthetic chlorinated paraffin according to claim 1, wherein: in the step S2, the liquid paraffin inside the chlorination reactor is stirred while the chlorination reactor is heated, and the rotation speed of the stirring device is 400-500 r/min.
4. The process for the production of the synthetic chlorinated paraffin according to claim 1, wherein: in the step S2, the chlorination reactor is in a sealed state.
5. The method for producing synthetic chlorinated paraffin according to claim 1, wherein: and in the step S4, chlorine gas is injected into the chlorination reactor, and simultaneously, a high-activity catalyst is injected into the chlorination reactor.
6. The method for producing synthetic chlorinated paraffin according to claim 1, wherein: the rotation speed of the stirring device in the step S5 is 300-400r/min, and the reaction time in the step S5 is 30 min.
7. The process for the production of the synthetic chlorinated paraffin according to claim 1, wherein: the stabilizer and the PH adjustor are injected into the chlorination reactor together while reducing the pressure and temperature in the step S6.
8. The process for the production of the synthetic chlorinated paraffin according to claim 1, wherein: the normal temperature in step S6 is 20 °, and the normal pressure in step S6 is 0.1 MPa.
CN202110244416.8A 2021-03-05 2021-03-05 Production method of synthetic chlorinated paraffin Pending CN115011378A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102145251A (en) * 2011-01-06 2011-08-10 鲁西化工集团股份有限公司氯碱化工分公司 Dechloridation device and process in chlorinated paraffin production process
CN103540361A (en) * 2012-07-12 2014-01-29 中国科学院大连化学物理研究所 Preparation method of chlorinated paraffin
CN106800948A (en) * 2015-11-25 2017-06-06 衡阳市骏杰化工有限公司 The method that catalytic chlorination produces chlorinated paraffin -52
CN110938470A (en) * 2019-11-15 2020-03-31 山东沾化阳光化学有限公司 Method for producing chlorinated paraffin-70 by low-temperature catalysis
CN111592913A (en) * 2020-05-21 2020-08-28 广州鑫泓设备设计有限公司 Chlorinated paraffin production process capable of improving utilization rate of raw material resources

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102145251A (en) * 2011-01-06 2011-08-10 鲁西化工集团股份有限公司氯碱化工分公司 Dechloridation device and process in chlorinated paraffin production process
CN103540361A (en) * 2012-07-12 2014-01-29 中国科学院大连化学物理研究所 Preparation method of chlorinated paraffin
CN106800948A (en) * 2015-11-25 2017-06-06 衡阳市骏杰化工有限公司 The method that catalytic chlorination produces chlorinated paraffin -52
CN110938470A (en) * 2019-11-15 2020-03-31 山东沾化阳光化学有限公司 Method for producing chlorinated paraffin-70 by low-temperature catalysis
CN111592913A (en) * 2020-05-21 2020-08-28 广州鑫泓设备设计有限公司 Chlorinated paraffin production process capable of improving utilization rate of raw material resources

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Application publication date: 20220906