CN102145251B - Dechloridation device and process in chlorinated paraffin production process - Google Patents
Dechloridation device and process in chlorinated paraffin production process Download PDFInfo
- Publication number
- CN102145251B CN102145251B CN 201110001947 CN201110001947A CN102145251B CN 102145251 B CN102145251 B CN 102145251B CN 201110001947 CN201110001947 CN 201110001947 CN 201110001947 A CN201110001947 A CN 201110001947A CN 102145251 B CN102145251 B CN 102145251B
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- CN
- China
- Prior art keywords
- hydrogen chloride
- dechloridation
- dechlorination
- liquid wax
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000012188 paraffin wax Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 41
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 33
- 239000001993 wax Substances 0.000 claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 20
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 claims abstract description 10
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000006298 dechlorination reaction Methods 0.000 claims description 36
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 18
- 239000000460 chlorine Substances 0.000 abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000011344 liquid material Substances 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 iron arene Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a dechloridation device and process in a chlorinated paraffin production process. The dechloridation process comprises the following steps: connecting a tail gas discharge pipe of a chlorination reaction kettle with a dechloridation kettle; introducing the chlorination tail gas produced by the chlorination reaction into hot liquid wax to perform a dechloridation reaction; eliminating the gas after the dechloridation reaction from a hydrogen chloride outlet; and eliminating the generated liquid material containing the liquid wax and using the eliminated liquid material containing the liquid wax as a raw material for continuous chlorination reactions. The process provided by the invention is a gas-gas two-phase material separation technology, can improve the chlorine utilization rate and the hydrogen chloride purity and remove impurities in the liquid wax and improve the product quality of chlorinated paraffin, and has tremendous economical benefits and practicability. By adopting the technology, the chlorine content in hydrogen chloride is less than or equal to 0.1%, the hydrogen chloride purity is improved to satisfy the use of a chlorosulfonic acid device; and meanwhile, the quality of liquid wax is improved, and the improvement of comprehensive quality of the product is facilitated.
Description
Technical field:
The present invention relates to remove in the chlorinated paraffin wax production process device and the technology of the chlorine in the hydrogen chloride gas.
Background technology:
In the chlorinated paraffin wax chlorination reaction process, there is part chlorine excessive, the one, cause chlorine consumption big, the 2nd, the reaction chlorinated exhaust needs to absorb with liquid caustic soda, increased production cost, the 3rd, pollute surrounding environment, hydrogen chloride can be sent to the chlorosulfonic acid device and produce chlorosulfonic acid, but purity, the chlorinity of chlorine are had relatively high expectations, and the hydrogen chloride that the conventional chlorinated paraffin wax mode of production is produced can not satisfy the production of chlorosulfonic acid.
Summary of the invention:
The objective of the invention is to overcome above-mentioned technical deficiency, and a kind of liquid wax dechlorination device and technology are provided.
Dechlorination device in a kind of chlorinated paraffin wax production process, the exhaust pipe of chlorination reaction still is communicated with the dechlorination still, the dechlorination still is connected with liquid wax input pipe, the hydrogen chloride outlet is established in the upper end of dechlorination still, the lower end links to each other with the chlorination reaction still by transfering material pump, and annular gas distributor and feed liquor tetrafluoro bend pipe are installed in the described dechlorination still.
The hydrogen chloride outlet of described dechlorination still upper end links to each other with the chlorosulfonic acid device.
Dechlorination process in a kind of chlorine paraffin production process, the chlorinated exhaust that chlorination reaction is produced feeds dechlorination reaction in the hot liquid wax, gas behind the dechlorination reaction is got rid of from the hydrogen chloride outlet, and the liquid that contains liquid wax of generation is got rid of the back as the raw material that continues chlorination reaction.
Successive reaction under described dechlorination reaction pressure 0.02-0.03MPa, temperature 70-90 ℃ and the light-initiated condition.
Gas behind the described dechlorination reaction enters the chlorosulfonic acid production system.
Liquid wax after the heating is squeezed in the dechlorination still continuously by certain flow, and the chlorinated exhaust with the generation in the chlorinated paraffin wax production process feeds the dechlorination still again.For improving removal effect, annular gas distributor and feed liquor tetrafluoro bend pipe are installed in still.Under certain pressure, temperature and light-initiated condition, purification hydrogen chloride gas and improve the quality of liquid wax.Contain hydrogen chloride, chlorine and steam in the chlorinated exhaust.Hydrogen chloride is emitted in chlorine in the tail gas, wax oil reaction, and chlorine is deviate from, and has improved the purity of tail gas hydrogen chloride; Because the still temperature is than higher, water vapor condensation is moisture in the tail gas, behind the absorbing hydrogen chloride, forms hydrochloric acid (concentration reaches more than 33%), is sunken to the bottom of wax oil automatically.Moisture in the wax oil is also because the temperature height is separated.Generate ferric trichloride behind iron ion and chlorine, the hcl reaction, because the density of ferric trichloride own is big, soluble in water, its solubility in wax oil is much smaller than the solubility in hydrochloric acid, so ferric trichloride is easy to be extracted from wax oil by hydrochloric acid.The reaction of aromatic hydrocarbons and chlorine, basic nitrogen and hydrogen chloride, product density is all greater than 1, and this moment, oily density was about 0.8, so be easy to be sunken to the bottom of wax oil, the bottom separator is discharged system by sewage draining exit, wax oil through so handling enters system again, has improved the purity of hydrogen chloride and liquid wax, is conducive to the lifting of product quality.
The present invention is two separating substances technology of gas gas, can improve the utilization rate of chlorine and the purity of hydrogen chloride gas, can remove the impurity in the liquid wax again, improves the product quality of chlorinated paraffin wax, has considerable economic and practicality.
The utilization of this technology makes content≤0.1% of chlorine in the hydrogen chloride, has improved hydrogen chloride gas purity to satisfy the use of chlorosulfonic acid device, improves the quality of liquid wax simultaneously, is conducive to the lifting of product comprehensive quality.
Description of drawings
Fig. 1 is apparatus of the present invention structure chart;
Fig. 2 is the structure chart of dechlorination still of the present invention;
Wherein: 1 chlorination reaction still, 2 dechlorination stills, 3 liquid wax input pipes, the outlet of 4 hydrogen chloride, 5 transfering material pumps, 6 annular gas distributors, 7 feed liquor tetrafluoro bend pipes, 8 circulating pumps
The specific embodiment
Dechlorination device in a kind of chlorinated paraffin wax production process communicates the exhaust pipe of chlorination reaction still 1 with dechlorination still 2, dechlorination still 2 is connected with liquid wax input pipe 3, and hydrogen chloride outlet 4 is established in the upper end of dechlorination still 2, and the lower end links to each other with chlorination reaction still 1 by transfering material pump 5.Annular gas distributor 6 and feed liquor tetrafluoro bend pipe 7 are installed in the described dechlorination still 2.
The hydrogen chloride of described dechlorination still 2 upper ends outlet 4 links to each other with the chlorosulfonic acid device.
Dechlorination process in a kind of chlorinated paraffin wax production process, the chlorinated exhaust that chlorination reaction is produced feeds dechlorination reaction in the hot liquid wax, gas behind the dechlorination reaction is got rid of from the hydrogen chloride outlet, and conduct continues the raw material of chlorination reaction after the liquid despumation that contains liquid wax of generation.
Step
1, liquid wax is squeezed in the dechlorination still.(90 ℃ of liquid wax temperature, flow 3m
3/ h, power is carried with centrifugal pump)
2, liquid wax liquid level is controlled 2/3rds in the dechlorination still.
3, feed chlorine from chlorination system through hydrogen.(50 ℃ of hydrogen chloride gas temperature, flow 500m
3/ h, pressure 0.02-0.06MPa)
4, in still, carry out dechlorination and other reactions: the chlorine in the tail gas, wax oil reaction, emit hydrogen chloride; Water vapor condensation is moisture, behind the absorbing hydrogen chloride, forms hydrochloric acid; Generate tri-chlorination behind iron ion and chlorine, the hcl reaction; The reaction of iron arene and chlorine, basic nitrogen and hydrogen chloride.(temperature 70-90 ℃, pressure 0.02-0.03MPa)
5, from dechlorination bottom removing impurities.
6, the liquid wax after will purifying with pump is squeezed into chlorination tank continuously and is carried out chlorination reaction.
7, the hydrogen chloride gas of Sheng Chenging is handled through gas purifications such as cyclone separator, cooler, filters.
8, hydrogen chloride gas is transported to the chlorosulfonic acid production system.(0 ℃ of hydrogen chloride gas temperature, flow 500m
3/ h, pressure 0.004MPa)
Claims (1)
1. the dechlorination device in the chlorinated paraffin wax production process, it is characterized in that, the exhaust pipe of chlorination reaction still is communicated with the dechlorination still, the dechlorination still is connected with liquid wax input pipe, the hydrogen chloride outlet is established in the upper end of dechlorination still, the lower end links to each other with the chlorination reaction still by transfering material pump, and annular gas distributor and feed liquor tetrafluoro bend pipe are installed in the dechlorination still; The hydrogen chloride outlet of described dechlorination still upper end links to each other with the chlorosulfonic acid device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110001947 CN102145251B (en) | 2011-01-06 | 2011-01-06 | Dechloridation device and process in chlorinated paraffin production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110001947 CN102145251B (en) | 2011-01-06 | 2011-01-06 | Dechloridation device and process in chlorinated paraffin production process |
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| Publication Number | Publication Date |
|---|---|
| CN102145251A CN102145251A (en) | 2011-08-10 |
| CN102145251B true CN102145251B (en) | 2013-07-17 |
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|---|---|---|---|
| CN 201110001947 Active CN102145251B (en) | 2011-01-06 | 2011-01-06 | Dechloridation device and process in chlorinated paraffin production process |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103170220B (en) * | 2013-04-01 | 2015-05-06 | 南京国威化工有限公司 | Continuous vacuum degassing process for chlorinated paraffin and device thereof |
| CN103289744B (en) * | 2013-06-14 | 2014-10-08 | 河北大景大搪化工设备有限公司 | Technique and device for continuously refining heavy liquid paraffin |
| CN104415580B (en) * | 2013-08-27 | 2016-04-27 | 丹阳市助剂化工厂有限公司 | A kind of liquid chlorinated paraffin dehydrochlorination and chlorine residue method and apparatus |
| CN104560197B (en) * | 2014-12-23 | 2016-06-15 | 丹阳市助剂化工厂有限公司 | The tail gas treatment process of chlorinated paraffin |
| CN105820841A (en) * | 2015-01-04 | 2016-08-03 | 丹阳市助剂化工厂有限公司 | Continuous vacuum degassing technology of chlorinated paraffin |
| CN106281459B (en) * | 2016-08-27 | 2018-05-11 | 山东聊城鲁西化工第六化肥有限公司 | A kind of system and technique for producing high viscosity chlorinated paraffin |
| CN107312567A (en) * | 2017-08-03 | 2017-11-03 | 江西塑星材料有限公司 | A kind of method of purification of chlorinated paraffin raw material wax oil |
| CN115011378A (en) * | 2021-03-05 | 2022-09-06 | 江苏国威化工有限公司 | Production method of synthetic chlorinated paraffin |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424381A (en) * | 2002-12-18 | 2003-06-18 | 宁波市镇海众利化工有限公司 | Devices for continuously producing chlorinated paraffin |
| CN100371425C (en) * | 2006-04-03 | 2008-02-27 | 上海氯碱化工股份有限公司 | Continuous production method of chlorinated paraffin |
| CN101544911B (en) * | 2009-05-06 | 2012-05-30 | 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 |
| CN201949806U (en) * | 2011-01-06 | 2011-08-31 | 鲁西化工集团股份有限公司氯碱化工分公司 | Dechlorination device in process of producing chlorinated paraffin |
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| CN102145251A (en) | 2011-08-10 |
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